Month: July 2021

Adding a certain compound to certain chemical reactions, such as: 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 19094-56-5, HPLC of Formula: C7H4ClIO2

Oxalylchloride (176 kg; 1386 mol; 1.14 eq) is added to a mixture of 2-chloro-5-iodo benzoic acid (343 kg; 1214 mol) (compound IX.1), fluorobenzene (858 kg) and N,N-dimethylformamide (2 kg) within 3 hours at a temperature in the range from about 25 to 30 C. (gas formation). After completion of the addition, the reaction mixture is stirred for additional 2 hours at a temperature of about 25 to 30 C. The solvent (291 kg) is distilled off at a temperature between 40 and 45 C. (p=200 mbar). Then the reaction solution (911 kg) is added to aluminiumchloride AlCl3 (181 kg) and fluorobenzene (192 kg) at a temperature between about 25 and 30 C. within 2 hours. The reaction solution is stirred at the same temperature for about an additional hour. Then the reaction mixture is added to an amount of 570 kg of water within about 2 hours at a temperature between about 20 and 30 C. and stirred for an additional hour. After phase separation the organic phase (1200 kg) is separated into two halves (600 kg each). From the first half of the organic phase solvent (172 kg) is distilled off at a temperature of about 40 to 50 C. (p=200 mbar). Then 2-propanole (640 kg) is added. The solution is heated to about 50 C. and then filtered through a charcoal cartouche (clear filtration). The cartouche may be exchanged during filtration and washed with a fluorobenzene/2-propanole mixture (1:4; 40 kg) after filtration. Solvent (721 kg) is distilled off at a temperature of about 40 to 50 C. and p=200 mbar. Then 2-propanole (240 kg) is added at a temperature in the range between about 40 to 50 C. If the content of fluorobenzene is greater than 1% as determined via GC, another 140 kg of solvent are distilled off and 2-propanole (140 kg) is added. Then the solution is cooled from about 50 C. to 40 C. within one hour and seeding crystals (50 g) are added. The solution is further cooled from about 40 C. to 20 C. within 2 hours. Water (450 kg) is added at about 20 C. within 1 hour and the suspension is stirred at about 20 C. for an additional hour before the suspension is filtered. The filter cake is washed with 2-propanole/water (1:1; 800 kg). The product is dried until a water level of <0.06% w/w is obtained. The second half of the organic phase is processed identically. A total of 410 kg (94% yield) of product which has a white to off-white crystalline appearance, is obtained. The identity of the product is determined via infrared spectrometry. 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, 2-Chloro-5-iodobenzoic acid, other downstream synthetic routes, hurry up and to see. Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2011/237526; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 61272-76-2, 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. 61272-76-2, name is 4-Fluoro-2-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 21 4-(((5-Fluoro-3-methyl-1H-indol-2-yl)methoxy)methyl)-N,N-dimethyl-1-phenylcyclohexanamine (one of two possible diastereomers) A mixture of Ain-12 (570 mg, 2 mmol), 4-fluoro-2-iodoaniline (Ian-04) (592 mg, 2.5 mmol), palladium(II) acetate (90 mg, 0.38 mmol), tetra-n-butylammonium chloride (564 mg, 2 mmol), triphenyl phosphine (203 mg, 0.80 mmol) and sodium carbonate (1.05 g, 10 mmol) was evacuated for 30 min in an oil pump. Anhydrous N,N-dimethyl formamide (15 ml), which had previously been flushed with argon for 1 h, was then added via a Schlenk attachment. The mixture was then stirred for 18 h at 100° C. The reaction mixture was then concentrated to small volume under vacuum. Toluene was repeatedly added to the residue, which was concentrated to small volume under vacuum each time and then divided between water and ethyl acetate (20 ml each). The phases were separated and the aqueous phase was extracted with ethyl acetate (3*30 ml). The combined organic phases were washed with 1 M sodium thiosultate solution (30 ml) and saturated sodium chloride solution (50 ml). The combined organic phases were dried with sodium sulfate and concentrated to small volume under vacuum. The crude product (1.06 g) was purified by MPLC [230 g, 46*3.6 cm, LiChroprep Si60 (15-25 mum)] with ethyl acetate/methanol (9:1). Yield: 319 mg (40percent), brown oil 1H-NMR (DMSO-d6): 1.25-1.70 (m, 7H); 1.90 (s, 6H); 2.21 (s, 3H); 2.56 (br d, 2H, J=11.9 Hz); 3.30 (d, 2H, J=6.3 Hz); 4.55 (s, 2H); 6.88 (ddd, 1H, J=9.5, 8.9, 2.6 Hz); 7.16-7.36 (m, 3H); 7.51-7.68 (m, 4H); 10.93 (s, 1H). 13C-NMR (DMSO-d6): 8.2; 24.4; 32.0; 36.9; 37.4; 58.5; 63.3; 74.8; 102.8 (d, J=23 Hz); 108.1; 109.0 (d, J=26 Hz); 111.8 (d, J=10 Hz); 126.1; 126.5; 127.2; 128.6 (d, J=12 Hz); 131.4; 131.9; 132.1; 132.2; 133.2; 133.9; 139.3; 156.5 (d, J=231 Hz).

The synthetic route of 4-Fluoro-2-iodoaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GRUNENTHAL GMBH; US2009/215725; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

68507-19-7, name is 3-Iodo-4-methoxybenzoic 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. category: iodides-buliding-blocks

3-iodo-4-methoxybenzoic acid (1.00 g, 7.19 mmol) was dissolved in SOCl2 (12.0 mL) and stirred at 80 C (22 h). Next, SOCl2 was removed in vacuo and azeotroped twice with benzene to give 57 (0.700 g, 2.36 mmol, 32%) as a white solid. 1H-NMR (400 MHz) CDC13: 8.50 (s, 1 H), 8.12-8.10 (d, 1 H), 6.88-6.86 (d, 1 H), 3.99 (s, 3 H); ,3C-NMR (100 MHz) CDC13: 165.1, 162.8, 141.9, 133.2, 126.3, 109.4, 85.2, 56.2.

The synthetic route of 68507-19-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; J-PHARMA CO., LTD.; WEMPE, Michael, F.; ENDOU, Hitoshi; WO2012/48058; (2012); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 401-81-0, Safety of 1-Iodo-3-(trifluoromethyl)benzene

Dioxane (100 mL) was purged with nitrogen gas for 10 min. Phenanthrolene ( 1.0 g) and copper (I) iodide (1.0 g) were added to the dioxane, the suspension was allowed to stir under a nitrogen atmosphere for 5 min, and then cesium carbonate ( 18.72 g, 57.45 mmol), dimethyl malonate (5.46 g, 50.6 mmol), and l-iodo-3-(trifluoromethyl)benzene (12.5 g, 46.0 mmol) were added. The reaction mixture was heated to reflux for 18 h and then cooled to room temperature. Aqueous 1 N HC1 was added to the reaction mixture, the layers were separated, and the aqueous layer was extracted with ethyl acetate (3 x 100 mL). The combined organic layers were dried over magnesium sulfate and filtered. Celite diatomaceous filter aid (5 g) was added to the filtrate, and the resulting suspension was concentrated under reduced pressure at 50 C to yield a solid consisting of the crude product adsorbed onto Celite. This solid was purified by silica gel chromatography eluting with a gradient of 100% hexanes to 25% ethyl acetate in hexanes to yield 7.36 g (58.0%) of the title product. NMR (CDC13) delta 7.59-7.65 (m, 3H), 7.49 (t, 1H), 4.70 (s, 1H), 3.76 (s, 6H).

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-3-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; ZHANG, Wenming; ANNIS, Gary David; WO2013/90547; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 628-21-7, name is 1,4-Diiodobutane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 1,4-Diiodobutane

Stage 1 (0244) An oven-dried 3 L 4-neck flask fitted with an internal thermometer, N2 bubbler, overhead stirrer and oven-dried mL pressure-equalising dropping funnel was charged with 1,4-dibromo-2,5-diethylbenzene (70 g, 240 mmol) and dry THF (700 mL). The solution was cooled with stirring to <-70 C. to produce a white slurry. s-Butyllithium (335 mL, 1.4 M, 465 mmol) was charged to the dropping funnel and added dropwise over the space of 1.5 h ensuring the reaction temperature did not exceed -70 C. The slurry was stirred for 3 h after which GCMS confirmed the lithiation was complete. The dropping funnel was charged with a solution of 1,4-diiodobutane (13.8 mL, 105 mmol) in dry THF (140 mL) which was then added dropwise over 0.75 h. The resulting slurry was allowed to warm to room temperature and stirred for 12 h. The reaction was quenched by addition of water. The mixture was transferred to a separating funnel and the layers were separated. The aqueous layer was extracted with diethyl ether and the combined organics were washed with water, dried with MgSO4, filtered and concentrated to yield an orange oil. The product was triturated with 500 mL methanol for 0.5 h and filtered as a white solid before being recrystallised from toluene/IPA to yield a white powder that was dried in the oven (24.21 g, 48%). GCMS indicated a purity of 96% and the material was taken to the next stage without further purification The synthetic route of 628-21-7 has been constantly updated, and we look forward to future research findings. Reference:
Patent; Cambridge Display Technology Limited; Sumitomo Chemical Company Limited; Kamtekar, Kiran; Steudel, Annette; (30 pag.)US9812644; (2017); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 31827-94-8, name: 2-Bromo-1-(4-iodophenyl)ethanone

General procedure: Sodium sulfite, sodium bicarbonate and sulfonyl chlorides in water were irradiated at 500 W for 20 min in a microwave oven. An ethanolic solution of the corresponding acetophenone was then added to sodium sulfinate and the reaction mixture was irradiated for 10 min to produce sulfones in good yields (1-13) (Scheme 2).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Paloque, Lucie; Bouhlel, Ahlem; Curti, Christophe; Dumtre, Aurelien; Verhaeghe, Pierre; Azas, Nadine; Vanelle, Patrice; European Journal of Medicinal Chemistry; vol. 46; 7; (2011); p. 2984 – 2991;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 620-05-3, name is (Iodomethyl)benzene, A new synthetic method of this compound is introduced below., Recommanded Product: 620-05-3

General procedure: In a flame-dried round-bottom flask, beta-amidoester (9) (1 mmol; 1 equiv) was taken in DMF (5 mL) at room temperature. To this reaction mixture KOt-Bu (1.2 mmol; 1.2 equiv) was added. After 5 minutes of stirring at same temperature alkyl halide (1.05 mmol; 1.05 equiv) was added and stirring was continued for 15 minutes. Upon completion of the alkylation (judged by TLC), it was diluted with 10 mL of EtOAc and quenched with water. The organic extracts were dried over anhydrous sodium sulphate and concentrated under vacuum. The crude product was purified by flash chromatography (hexane and EtOAc as eluents) to afford compounds 10.

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:
Article; Kumar, Nivesh; Ghosh, Santanu; Bhunia, Subhajit; Bisai, Alakesh; Beilstein Journal of Organic Chemistry; vol. 12; (2016); p. 1153 – 1169;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 4028-63-1, A common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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.

tert-Butyllithium (9.0 mL of a 1.7 mol/l solution in n-pentane, 15.3 mmol)was added to iodomesitylene (10) (1.51 g, 6.14 mmol) in Et2O (20 mL) at ?78 °C under inertatmosphere. After 30 min, CuCN (273 mg, 3.07 mmol) was added and the suspension stirred at?60 °C for 2 h. The reaction mixture was then treated with nitrobenzene (0.94 mL, 9.12 mmol)and allowed to warm up to room temperature overnight. An aqueous solution of NH3 (12.5percentw/w, 80 mL) was slowly added and the resulting residue was extracted with MTBE (3 x 50 mL).The combined organic layers were washed with water (50 mL) and brine (50 mL), dried overMgSO4, filtered, and the solvent was removed in vacuum. The product 11 could be obtained aftercolumn chromatography (SiO2, n-hexane, Rf 0.43) as a colorless solid (542 mg, 2.27 mmol,74percent), mp 98 °C (ref.27 99?100 °C). 1H NMR (300 MHz, CDCl3): delta 6.94 (s, 4 H), 2.34 (s, 6 H),1.87 (s, 12 H) ppm. 13C{1H} NMR (75 MHz, CDCl3): delta 137.0 (2 C), 136.0 (2 C), 135.5 (4 C),128.2 (4 CH), 21.1 (2 CH3), 19.8 (4 CH3) ppm. IR (ATR): 2997 (w), 2938 (m), 2916 (m), 1470(m), 1436 (m), 1375 (m), 1004 (m), 852 (s), 595 (m) cm?1. MS (EI, 70 eV), m/z (percent): 238 (99)[M+], 223 (100), 208 (33), 193 (25). Anal. calcd. for C18H22 (238.37): C 90.70, H 9.30; found C90.73, H 9.34.

The synthetic route of 4028-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Behler, Florian; Wickleder, Mathias S.; Christoffers, Jens; ARKIVOC; vol. 2015; 2; (2014); p. 64 – 75;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 624-75-9, 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. 624-75-9, name is 2-Iodoacetonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 7-BENZYLOXYMETHYL-8- (4-HYDROXYPHENYL)-1, 3-DIPROPYL-1, 3,7- trihydropurine-2,6-dione (LG, 2. 2MMOL) in tetrahydrofuran (20ML) was added potassium t- butoxide (0.28g, 2. 4MMOL), and the mixture stirred for 30 minutes at room temperature. IODOACETONITRILE (0. 38G, 2. 23MMOL) was then added, and the mixture stirred for 16 hours at room temperature. The solvent was removed under reduced pressure, and the residue was dissolved in ethyl acetate and passed through a silica gel plug, to provide 7-BENZYLOXYMETHYL-8- (4- cyanomethoxyphenyl)-1, 3-dipropyl-1, 3,7-trihydropurine-2, 6-dione, a compound of formula (7)

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, 2-Iodoacetonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CV THERAPEUTICS, INC.; WO2004/106337; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 19099-54-8, 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. 19099-54-8, name is 1-Iodo-2-isopropylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

0.3 mmol of sodium carbonate, 0.1 mmol of 1,2-bis(3-methoxyphenyl)acetylene, 0.005 mmol of palladium acetate, and double (2-0.005 mmol of diphenylphosphoryl phenyl)ether, 0.15 mmol of pinacol borate, 0.15 mmol of 2-isopropyliodobenzene and N,N-1 mL of methylformamide was added to a 15 mL reaction tube, nitrogen was repeatedly filled 10 times, placed in an oil bath at 120 C, and reacted for 24 hours;Cool to room temperature, dilute with ethyl acetate, wash three times with water, dry with organicNa2SO4 is dried, filtered, concentrated, thin layerChromatography purification gave 20.8 mg of the desired product in a yield of 43%. The nuclear magnetic and high resolution mass spectra of this compound are characterized as follows:

The chemical industry reduces the impact on the environment during synthesis 1-Iodo-2-isopropylbenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Huaqiao University; Cheng Guolin; Lv Weiwei; (10 pag.)CN109879899; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com