Tag: M.W=200-300

Related Products of 19099-54-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 19099-54-8, name is 1-Iodo-2-isopropylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of N,7-[(benzothiazol-2-yl)-9,9-diethylfluoren-2-yl)-N-(2,6-diisopropylphenyl)amine (Example 19; 4.24 g, 8 mmol), 2-isopropyl iodobenzene (12.3 g, 50 mmol), 18-crown-6 (0.169 g), copper powder (1 g, 15.7 mmol) and potassium carbonate (4.41 g, 32 mmol) was kept at 240 C. for 4 hours under nitrogen, cooled, diluted with toluene and filtered. The filtrate was washed with water, dried and concentrated. The residue (15.32 g) was chromatographed over silica gel. The column was eluted with 1:1 toluene to get the product, and the product was crystallized from a mixture of isopropanol and toluene, 3.85 g (74%), m.p. 259.3-262.9 C. Mass spec: m/z 648 (M+). Anal. Calcd. for C45H48N2S: C, 83.29; H, 7.46; N, 4.32 and S, 4.94%. Found: C, 83.33; H, 7.45; N, 4.31 and S, 4.96%. 1H NMR (CDCl3) delta ppm: 0.29, 0.32 (2t, 6H, 7.28, 7.36 Hz), 0.75 (broad envelope 6H), 1.18 (broad, 12H), 1.90 (m, 2H), 2.08 (m, 2H), 3.20 (broad s?, 2H), 3.35 (m, 1H), 6.58 (m, 1H), 6.81 (dd, 1H, 1.32 and 7.88 Hz), 7.08 (m, 2H), 7.23 (m, 3H), 7.34 (m, 3H), 7.47 (m, 2H), 7.62 (d, 1H, 7.92 Hz), 7.88 (d, 1H, 7.88 Hz), 7.99 (m, 2H). 13C NMR delta ppm: 8.33, 8.60, 21.46, 23.85, 27.66, 28.00, 28.57, 32.50, 32.90, 56.55 (10 sp3C), 118.89, 119.76, 120.75, 121.30, 121.49, 122.87, 124.27, 124.85, 125.30, 125.78, 126.22, 126.43, 127.18, 127.87, 128.23, 129.04, 130.86, 132.95, 134.91, 142.58, 142.88, 143.53, 145.02, 148.05, 148.19, 150.06, 151.86, 152.06, 154.29 and 169.02 (30 sp2C).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-Iodo-2-isopropylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; The United States of America, as represented by the Secretary of the Air Force; Tan, Loon-Seng; Kannan, Ramamurthi; (43 pag.)US10113065; (2018); B1;,
Iodide – Wikipedia,
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Application of 455-13-0, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 455-13-0, name is 4-Iodobenzotrifluoride belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a solution of aryl iodide (10 mmol, 1.0 equiv.) in THF (10 mL, 1.0 M) was added 2-propyn-1-ol (1.24 mL, 1.2 equiv.), diisopropylamine (1.68 mL, 1.2 equiv.), PdCl2(PPh3)2 (0.3 mmol, 3 mol%) andCuI (0.5 mmol, 5 mol%). The resulting solution changed colour from yellow to orange and finallybrown in two minutes. The reaction mixture was heated at 50 C and stirred until completeconsumption of the aryl iodide was observed (tlc, 2 h). After filtering the crude material over a padof silica (5 g) and evaporation of the solvent the crude material (1H-NMR) was purified by silica column chromatography (eluent 10% EtOAc in pentanes, Rf = 0.41). After removal of the volatiles,the desired hydroxyl product was typically isolated as yellow oil with a purity > 98% (by 1H-NMR)and was used directly in the next step. Copies of NMR spectra are provided in the electronicsupplementary information.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 4-Iodobenzotrifluoride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Donnelly, Kian; Zhang, Huan; Baumann, Marcus; Molecules; vol. 24; 20; (2019);,
Iodide – Wikipedia,
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Reference of 124700-41-0, These common heterocyclic compound, 124700-41-0, name is 2-Fluoro-5-iodobenzoic acid, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Preparation 29 Ethyl 3-(2-fluoro-5-iodophenyl)-3-oxopropanoate To a stirred solution of 5.32 g of 2-fluoro-5-iodobenzoic acid from Preparation No. 28 in 20 mL of THF, under argon, is added 3.9 g of carbonyldiimidazole. In a separate flask, 2.8 mL of chlorotrimethylsilane is added to a mixture of 3.74 g of potassium ethyl malonate in 20 mL of acetonitrile. The mixture is stirred under argon for 18 h, then cooled to 0 C. for the dropwise addition of 6.6 mL of DBU. The mixture is stirred for 3 h at 0 C., then the solution of acyl imidazolide prepared above is added via cannula. After 2 h, the mixture is partitioned between ether and excess dilute HCl, and the organic phase is washed with dilute HCl and brine and dried (MgSO4). Removal of the solvent under reduced pressure left a colorless oil, which is flash chromatographed on silica using 10% ethyl acetate in hexane to provide 5.07 g of the title compound as dense pinkish prisms. Physical properties as follows: 1H NMR (CDCl3) delta1.34, 4.27, 5.82, 6.89, 7.7, 8.2 ppm; IR 1624, 1485, 1419, 1245, 1193, 1070, 1028, 813 cm-1.

Statistics shows that 2-Fluoro-5-iodobenzoic acid is playing an increasingly important role. we look forward to future research findings about 124700-41-0.

Reference:
Patent; Pharmacia & Upjohn Company; US6248739; (2001); B1;,
Iodide – Wikipedia,
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Synthetic Route of 83171-49-7, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 83171-49-7 name is 3-Chloro-5-iodoaniline, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

General procedure: The corresponding pyrazinoic acid (5.0 mmol) was dispersed in dry toluene (20 mL) and mixed with 1.5eq. of thionyl chloride (0.55 mL, 7.5 mmol). The reaction mixture was heated to reflux for approximately 1 h. Next, the excess of thionyl chloride was removed by repeated evaporation with dry toluene under vacuum.The crude acyl chloride was dissolved in dry acetone(20 mL) and added drop-wise to a stirred solution of the corresponding aniline (5.0 mmol) with triethylamine(5.0 mmol) in dry acetone (30 mL). The reaction mixture was stirred at ambient temperature for up to 6 h. The completion of the reaction was monitored by TLC (eluent: hexane/ethyl acetate; r =2 : 1). The crude product adsorbed on silica gel by solvent evaporation was purified by flash chromatography(hexane/ethyl acetate gradient elution).The analytical data of the prepared compounds were fully consistent with the proposed structures and are available in the Supplementary Data.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Chloro-5-iodoaniline, and friends who are interested can also refer to it.

Reference:
Article; Zitko, Jan; Barbora, Servusova-Vanaskova; Paterova, Pavla; Navratilova, Lucie; Trejtnar, Frantisek; Kunes, Jiri; Dolezal, Martin; Chemical Papers; vol. 70; 5; (2016); p. 649 – 657;,
Iodide – Wikipedia,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 32024-15-0, name is 3-Iodo-4,5-dimethoxybenzaldehyde, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 3-Iodo-4,5-dimethoxybenzaldehyde

3, 4-dimethoxy-5-iodo-benzaladehyde (2.92 g, 10 mmol) wasdissolved in minimal EtOH and stirred in an ice bath. After the entire solid had dissolved NaBH4 (3.4 g,~10 mmol) was added to the mixture. The progress was monitored by HPLC. After, 1.5 hours thecomplete reaction mixture was concentrated under vacuum to half its volume and poured into aseparating funnel containing water. Aqueous layer was extracted three times with DCM. It was thenconcentrated to give the final product as yellow oil (2.79 g, 9.5 mmol). 1H NMR (300 MHz, DMSO-d6): 7.40 – 7.27 (m, 1H), 7.02 (d, J = 1.7 Hz, 1H), 4.53 (s, 2H), 3.87 (s, 3H), 3.77 (s, 3H). UV-Vis: 214.7, 285.1nm.

According to the analysis of related databases, 32024-15-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Maresh, Justin J.; Ralko, Arthur A.; Speltz, Tom E.; Burke, James L.; Murphy, Casey M.; Gaskell, Zachary; Girel, Joann K.; Terranova, Erin; Richtscheidt, Conrad; Krzeszowiec, Mark; Synlett; vol. 25; 20; (2014); p. 2891 – 2894;,
Iodide – Wikipedia,
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52548-63-7, name is 5-Fluoro-2-iodobenzoic acid, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Product Details of 52548-63-7

To a solution of 1H-pyrrolo[2,3-c]pyridine (70 g, 0.59 mol) in MeOH (1,050 mL) and H2O (350 mL) was added KOH (83 g, 1.48 mol) and tert-butyl 3-oxopiperidine-1- carboxylate (259 g, 1.30 mol). The resulting mixture was stirred at 75-80 oC (oil bath temperature) for 18 h. The reaction mixture was concentrated under reduced pressure to remove MeOH, then H2O (700 mL) was added and the mixture was extracted with EtOAc (3 ¡Á 1000 mL). The organic layers were filtered and the filtered cake was washed with EtOAc (2 ¡Á 150 mL) to afford tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,4- dihydropyridine-1(2H)-carboxylate (75 g, 42% yield) as white solid. The organic layer was concentrated under reduced pressure to about 250 mL. The residue was stirred at 5-9 oC for 18 h. The residue was filtered and the filtered cake was washed with EtOAc (2 ¡Á 60 mL) to give a mixture of tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,6- dihydropyridine-1(2H)-carboxylate and tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,4- dihydropyridine-1(2H)-carboxylate (1:3.5 via LCMS; (28 g, 16% yield) as white solid. tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,4-dihydropyridine-1(2H)- carboxylate: Yield: 75 g (42%); Rt value: 0.570 (LCMS Method C); (M+H)+ = 300.1; 1H NMR (MeOD, 400 MHz): delta ppm 8.65-8.70 (d, J = 2.8 Hz, 1H), 8.05-8.15 (d, J = 5.6 Hz, 1H), 7.70-7.90 (m, 1H), 7.54 (s, 1H), 7.35-7.50 (m, 1H), 3.60-3.75 (m, 2H), 2.50-2.60 (t, J = 5.6 Hz, 2H), 2.00-2.10 (m,2H), 1.55-1.60 (m, 9H). Mixture of tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,6-dihydropyridine- 1(2H)-carboxylate and tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,4-dihydropyridine- 1(2H)-carboxylate: Rt value: 0.568 (LCMS Method C); (M+H)+ = 300.1. A suspension of tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,4-dihydropyridine- 1(2H)-carboxylate and tert-butyl 5-(1H-pyrrolo[2,3-c]pyridin-3-yl)-3,6-dihydropyridine- 1(2H)-carboxylate (1 g, 3.34 mmol, ~10:1 ratio of isomers), 5-fluoro-2-iodobenzoic acid (977 mg, 3.67 mmol), K2CO3 (1.15 g, 8.33 mmol), CuI (63 mg, 0.334 mmol) and 1,10- phenanthroline (60 mg, 0.334 mmol) in DMF (13 mL, 0.26 M reaction concentration) was degassed with N2 for 15 min. The reaction mixture was then placed under N2 and heated to 70 oC for 24 h. The reaction was then cooled to room temperature and filtered through a plug of Celite using a small amount of DMF to rinse the filter cake. The DMF solution was cooled to 0 oC and a 1N aq. HCl solution (~10 mL) was added, maintaining a pH of ~5, followed by the addition of H2O (~10 mL) and EtOAc for the extraction. The EtOAc layer was separated and the aqueous layer (pH~5) was extracted three additional times with EtOAc. The EtOAc layers were combined and washed with H2O followed by brine. After drying over Na2SO4, the EtOAc layer was evaporated and the resulting residue was dried under high vacuum overnight to afford ~2 grams of crude 2-(3-(1-(tert-butoxycarbonyl)-1,4,5,6-tetrahydropyridin-3-yl)-1H-pyrrolo[2,3-c]pyridin- 1-yl)-5-fluorobenzoic acid and 2-(3-(1-(tert-butoxycarbonyl)-1,2,5,6-tetrahydropyridin-3- yl)-1H-pyrrolo[2,3-c]pyridin-1-yl)-5-fluorobenzoic acid (>10:1 ratio of isomers). The crude material was used directly for the next step without further purification. LCMS: 5.748 min (LCMS Method G): 438.47 (M + 1).1H NMR (400 MHz, CDCl3): delta 8.52-8.48 (m, 1H), 8.20-8.15 (m, 1H), 8.07 (bs, 1H), 8.01 (s, 1H), 7.85 (d, 1H, J = 8.4 Hz), 7.76 (s, 1H), 7.55 (bs, 1H), 7.42 (d, 1H, J = 5.2 Hz), 3.67 (bs, 2H), 2.50-2.47 (m, 2H), 2.06-2.01 (m, 2H), 1.54 (s, 9H). To a solution of the crude mixture from Step 2, (3.34 mmol), N-methylpropan-2- amine (731 mg, 10.02 mmol) and iPr2NEt (1.74 mL, 10.02 mmol) in EtOAc (9 mL) was added a 50 wt% solution of T3P in EtOAc (6 mL, 10.02 mmol) dropwise at ~10 oC. The reaction was stirred for 2 h, cooled to 0 oC, and a 1N aq. NaOH solution (~10 mL) was slowly added. The EtOAc layer was separated and the aqueous layer was extracted twice with EtOAc. The EtOAc layers were combined and washed with sat. NH4Cl, H2O, and then brine. After drying over Na2SO4, the EtOAc layer was evaporated to afford 1.65 grams of crude tert-butyl 5-(1-(4-fluoro-2-(isopropyl(methyl)carbamoyl)phenyl)-1H- pyrrolo[2,3-c]pyridin-3-yl)-3,4-dihydropyridine-1(2H)-carboxylate (purity: ~90% based on LCMS analysis). This material was used directly for the next step without further purification. LCMS: 6.247 min (LCMS Method G); 493.55 (M+1).1H NMR (400 MHz, CDCl3) The title compound was observed as a mixture of rotamers by NMR, the major rotamer isomer peaks were tabulated and are provided: delta 8.07-8.68 (m, 1H), 8.35-8.32 (m, 1H), 7.88 (d, 1H, J = 5.2 Hz), 7.62 (bs, 1H), 7.55-7.52 (m, 1H), 7.43-7.41 (m, 1H), 7.29-7.18 (m, 2H), 4.65-4.75 (m, 1H), 3.60-3.65 (m, 2H), 2.69 (s, 3H), 2.40-2.45 (m, 2H), 1.90-2.00 (m, 2H), 1.57 (s, 9H), 0.95-0.94 (m, 3H), 0.56-0.59 (m, 3H).

The synthetic route of 52548-63-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; VITAE PHARMACEUTICALS, INC.; CACATIAN, Salvacion; CLAREMON, David A.; DONG, Chengguo; FAN, Yi; JIA, Lanqi; LOTESTA, Stephen D.; SINGH, Suresh B.; VENKATRAMAN, Shankar; YUAN, Jing; ZHENG, Yajun; ZHUANG, Linghang; (285 pag.)WO2018/53267; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 452-79-9,Some common heterocyclic compound, 452-79-9, name is 2-Fluoro-1-iodo-4-methylbenzene, molecular formula is C7H6FI, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

A mixture of 3-fluoro-4-iodotoluene (2.26 g, 9.58 mmol), N-bromosuccinimide (2.03 g, 11.49 mmol) and benzoyl peroxide (5 mol %, 116 mg, 0.48 mmol) in carbon tetrachloride (5 ml) was stirred at reflux for 20 hours, cooled, diluted with dichloromethane and filtered. The purple coloured filtrate was washed with saturated sodium thiosulphate solution (aq) (20 ml). The organic layer was separated, dried over sodium sulphate and the solvent removed by rotary evaporation to give the title compound as a yellow oil (2.58 g, 86%).1H-NMR (250 MHz, CDCl3): delta 7.72 (1H, m), 7.11 (1H, m), 6.94 (1H, m), 4.41 (2H, s).

The synthetic route of 452-79-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; US2010/137276; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 25309-64-2,Some common heterocyclic compound, 25309-64-2, name is 1-Ethyl-4-iodobenzene, molecular formula is C8H9I, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Example 1Preparation of pinacol ester of 4-ethylphenylboronic acid In a 2 necks Schlenk type flask, provided with a magnetic stirring bar and topped by a coolant, 4-ethylbenzene iodide (0.232 g, 1 mmol), pinacolborane (0.128 g, 1 mmol) and triethylamine (59 mg, 1 mmol) are added to 10 ml of a distilled THF solution containing magnesium turnings (24 mg, 1 mmol). The reactive mixture is stirred for approximately 15 hours at THF reflux.At the end of the reaction, the crude reaction product is hydrolyzed by 20 ml of neutral water and extracted by diethyl ether (3¡Á40 ml). The joined organic phases are washed by 2¡Á50 ml of neutral water then dried on MgSO4. After solvent evaporation, the obtained yield is of 96% with a total conversion of the starting iodide (yield/conversion of 96%). The resulting boronic ester is analyzed by GC, NMR 1H and 13C and GC/MS.Characterizations:NMR 1H, 7.74 (2H, D, 3 Hz); 7.22 (2H, D, 3 Hz); 2.66 (2H, Q, 3 Hz); 1.34 (12H, s); 1.24 (3H, T, 3 Hz).NMR 13C, 146.68; 133.87; 127.23; 126.31; 82.58; 28.08; 23.82; 14.42.Mass spectrometry: 232-231 (M+, 6-2%); 217-216 (8-2%); 147 (19%); 146-145 (71-15%); 134 (17%); 133 (100%); 132-131 (63-21%); 118 (18%); 117 (51%); 116-115 (17-4%); 105 (18%); 104 (10%); 91 (11%); 85 (14%); 77-76 (9-2%).Ultimate Analyses:calculated %: C: 72.44%; H: 9.12%; B: 4.66%.obtained %: C: 70.22%; H: 9.25%; b: 4.39%.

The synthetic route of 25309-64-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Universite De Nice Sophia Antipolis; US2011/282090; (2011); A1;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 608-28-6, name is 2-Iodo-1,3-dimethylbenzene, molecular formula is C8H9I, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Safety of 2-Iodo-1,3-dimethylbenzene

General procedure: To a reaction tube containing (17alpha-20E)-21-(tri-n-butylstannyl)-19-norpregna-1,3,5(10)20-tetraene-3,17beta-diol, 2a, were added a few crystals of 2,6 di-tert-butyl-4-methylphenol and the substituted phenyl/xylyl iodide. The tube was dried under vacuum for 24 h, then exchanged with argon at least four times. Tetrakis(triphenylphosphine) palladium (0) (0.024 g, 0.02 mmol) and dried, degassed toluene (5 mL) were added and the reaction was heated at 110 C for 6-18 h. After cooling to room temperature, the reactuib mixture was transferred to a flask with ethyl acetate (50 mL), activated charcoal was added, the mixture heated to boiling, and then filtered through a Celite pad. To the filtrate containing the substituted phenyl vinyl estradiol derivative, fluorsil (4-8 g) was added and then mixture was evaporated to dryness. Hexane was then added to the slurry and the mixture was again evaporated to dryness. The substituted phenyl vinyl estradiol was isolated using flash chromatography and characterized by 1H and 13C NMR, elemental analysis

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 608-28-6, its application will become more common.

Reference:
Article; Hanson, Robert N.; McCaskill, Emmett; Tongcharoensirikul, Pakamas; Dilis, Robert; Labaree, David; Hochberg, Richard B.; Steroids; vol. 77; 5; (2012); p. 471 – 476;,
Iodide – Wikipedia,
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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, A new synthetic method of this compound is introduced below., HPLC of Formula: C3H4F3I

Zn/Cu couple (0.6 g, 9.23 mmol), 1,1,1-trifluoro-3-iodopropane (1.37 g, 6.11 mmol, Aldrich), benzene (16 mL), and N,N-dimethylformamide (1 mL) were heated together for 3 hr at 60 C. under N2. The t-butyl ester pyran from Part A (1.0 g, 2.04 mmol) and [1,1?-Bis(diphenylphosphino)ferrocene]dichloropalladium(II), complex with CH2Cl2 (1:1) (0.083 g, 0.102 mmol, Aldrich) were added, and the resulting dark mixture was stirred overnight at 69 C. under N2. Zn/Cu couple (0.6 g, 9.23 mmol), 1,1,1-trifluoro-3-iodopropane (1.37 g, 6.11 mmol, Aldrich), benzene (16 mL), and N,N-dimethylformamide (1 mL) were heated together for 3 hr at 60 C. under N2. This mixture was added to the original flask, and the resulting mixture was stirred overnight at 70 C. under N2. An additional portion of the Pd catalyst (same amount used above) was added to the mixture, and the resulting mixture was stirred at 70 C. overnight under N2. Zn/Cu couple (0.6 g, 9.23 mmol), 1,1,1-trifluoro-3-iodopropane (1.37 g, 6.11 mmol, Aldrich), benzene (16 mL), and N,N-dimethylformamide (1 mL) were heated together for 3 hr at 60 C. under N2. This mixture was added to the original flask along with another portion of the Pd catalyst (same amount used above), and the resulting mixture was stirred overnight at 70 C. under N2. The mixture was allowed to cool to ambient temperature, and 50 mL each of saturated NH4Cl(aq) and deionized water were added to the mixture. The mixture was then stirred for 15 min. Afterward, the mixture was further diluted with 200 mL of ethyl acetate and filtered through a pad of Celite . The filter cake was washed with 50 mL each of deionized water and ethyl acetate. The layers were separated, and the organic layer was washed with 100 mL of saturated NaCl(aq), dried over MgSO4, and concentrated in vacuo to form a brown oil (1.43 g). Chromatography (silica, ethyl acetate/hexanes) afforded 0.80 g (78% yield) of a yellow oil.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Barta, Thomas E.; Becker, Daniel P.; Bedell, Louis J.; Boehm, Terri L.; Brown, David L.; Carroll, Jeffery N.; Chen, Yiyuan; Fobian, Yvette M.; Freskos, John N.; Gasiecki, Alan F.; Grapperhaus, Margaret L.; Heintz, Robert M.; Hockerman, Susan L.; Kassab, Darren J.; Khanna, Ish K.; Kolodziej, Stephen A.; Massa, Mark A.; McDonald, Joseph J.; Mischke, Brent V.; Mischke, Deborah A.; Mullins, Patrick B.; Nagy, Mark A.; Norton, Monica B.; Rico, Joseph G.; Schmidt, Michelle A.; Stehle, Nathan W.; Talley, John J.; Vernier, William F.; Villamil, Clara I.; Wang, Lijuan J.; Wynn, Thomas A.; US2005/9838; (2005); A1;,
Iodide – Wikipedia,
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