Tag: M.W=300-400

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. 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, A new synthetic method of this compound is introduced below., Quality Control of Methyl 5-bromo-2-iodobenzoate

A magnetically stirred and degassed mixture of compound 5 (1.39 g, 20.8 mmol), compound 37 (6.45 g, 18.9 mmol), Cul (359 mg, 1.9 mmol), 1 , 10-phenanthroline (680 mg, 3.8 mmol) and Cs2C03 (9.30 g, 28.4 mmol) in anhydrous toluene (40 mL) was heated at 100 C under a nitrogen atmosphere for 48 h. The cooled reaction mixture was then passed through a pad of TLC-grade silica and the filtrate concentrated under reduced pressure. The residue so formed was subjected to flash chromatography (silica, 30: 1 v/v hexane/ethyl acetate elution) to afford, after concentration of the appropriate fractions (Rf = 0.5 in 8: 1 v/v hexane/ethyl acetate), compound 38 (5.21 g, 99%) as a clear, colorless syrup. (0734) 1H NMR (400 MHz, CDCI3) £ 7.85 (d, J = 2.4 Hz, l H), 7.59 (dd, J = 8.5 and 2.4 Hz, 2H), 7.18 (m, 1H), 6.71 (m, 2H), 6.25 (m, 2H), 3.65 (s, 3H). (0735) 13C NMR (100 MHz, CDC13) delta 166.1 , 139.4, 135.3, 133.5, 129.4, 128.3, 122.0, 120.5, 1 10.2, 52.8. (0736) IR vmax 2950, 1729, 1594, 1563, 1498, 1435, 1400, 1329, 1288, 1267, 1238, 1 123, 1094, 1015, 966, 922, 826, 727 cm 1. (0737) MS (ESI, +ve): m/z 282 and 280 [(M+H) , both 50%], 250 and 248 (96 and 100). (0738) HRMS (ESI, +ve) Found: (M i l ) . 279.9972. C12Hi179BrN02 requires (M i l ) . 279.9973.

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; THE AUSTRALIAN NATIONAL UNIVERSITY; BANWELL, Martin Gerhardt; ZHANG, Yiwen; (159 pag.)WO2017/100819; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

364-12-5, name is 5-Bromo-2-iodobenzotrifluoride, 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. Recommanded Product: 364-12-5

[0088] Step A: Preparation of 1 -(4-bromo-2-(trifluoromethyl)phenyl)-2,2-dimethylpropan- 1-one [0089] 4-Bromo-1-iodo-2-(trifluoromethyl)benzene(2.0 g, 5.70 mmol, 1.0 equiv) was placed in an oven-dried scintillation vial and dissolved in THF (11.4 mL). Isopropylmagenesium chloride lithium chloride complext (5.7 mL of a 1.3 M solution in ether, 7.41 mmol, 1.3 equiv) was added, and the resultant dark brown solution was stuffed at rt for 2 h. The Grignard solution was then added dropwise to a solution of trimethylacetyl chloride (0.893 g, 7.41 mmol, 1.3 equiv in 11 mL THF) and the reaction was stuffed overnight. The reaction was quenched carefully with sat. NH4C1, diluted with ethyl acetate and water, and the layers were separated. The aqueous layer was extracted with ethylacetate (xl) and the combined organics were washed with brine, dried over sodium sulfate, filtered and concentrated. Purification by silica gel chromatography eluting with a 5% ethyl acetate/hexane gradient afforded 1.05 g (3.40 mmol, 60% yield) of the title compound as a yellow oil. ?H NMR (400 MHz, CDC13) oe 7.83 (d, J= 1.9 Hz, 1H), 7.69 (ddd, J= 8.3, 1.9, 0.7 Hz, 1H), 7.17 (d, J= 8.2 Hz, 1H), 1.25 (s, 9H); ?3C NMR (126 MHz, CDC13) oe 211.1, 138.3, 134.3, 130.1 (q, J= 4.5 Hz), 126.9, 123.7, 122.8, 121.5, 44.7, 27.6; ESIIVIS m/z 310 [M+Hf?.

The synthetic route of 364-12-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DOW AGROSCIENCES LLC; LOSO, Michael R.; GUSTAFSON, Gary D.; KUBOTA, Asako; YAP, Maurice C.; BUCHAN, Zachary A.; STEWARD, Kimberly M.; SULLENBERGER, Michael T.; HOEKSTRA, William J.; YATES, Christopher M.; WO2015/160664; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 328-73-4, name is 1-Iodo-3,5-bis(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 328-73-4, category: iodides-buliding-blocks

General procedure: To a test tube containing a magnetic bar was added aryl halide (1.0 mmol), CuCl2 (13.4 mg, 0.1 mmol), KOH (336 mg, 6.0 mmol), ethylene glycol(12 muL, 0.2 mmol), and DMSO/H2O (1.0 mL/0.5 mL). After flushing with argon, the mixture was stirred in a preheated oil bath at 120 °C for 24 h. After cooled to ambient temperature, the reaction mixture was distributed in aqueous HCl (5 percent) and ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous MgSO4, and concentrated under vacuum. The crude product was further purified by column chromatography (EtOAc/n-Hexane) to provide the phenols.

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; Kim, Jihye; Battsengel, Oyunsaikhan; Liu, Yajun; Chae, Junghyun; Bulletin of the Korean Chemical Society; vol. 36; 12; (2015); p. 2833 – 2840;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 148836-41-3,Some common heterocyclic compound, 148836-41-3, name is 1-Bromo-4-chloro-2-iodobenzene, molecular formula is C6H3BrClI, 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.

Step D: Preparation of l -Bromo-4-chloro-2-(3,3,3- triethoxyprop- 1 -yny l)benzene; [0835] A suspension of l -bromo-4-chloro-2-iodobenzene (2.5 g, 7.9 mmol), 3,3,3-triethoxyprop-l-yne (2.4 g, 13.9 mmol), copper(I) iodide, (455 mg, 2.3 mmol), and trans-dichlorobis(triphenylphosphine)palladium(II) (559 mg, 0.79 mmol) was treated with ACN (30 mL). The reaction was capped, evacuated under vacuum, backfilled with argon, and treated with TEA (9.9 mL, 71.6 mmol). The reaction was stirred at 23C. After 2 hours, the reaction mixture was concentrated in vacuo to remove all solvents, diluted with EtOAc (250 mL) and washed with brine (150 mL), dried over MgSO4, concentrated in vacuo and purified by silica gel chromatography (eluant: 4% EtOAc/hexane + 1%TEA), affording 2.6 g of l-bromo-4-chloro-2-(3,3,3-triethoxyprop-l- ynyl)benzene.

The synthetic route of 148836-41-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AMGEN INC.; WO2008/76427; (2008); A2;,
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. 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C6H3BrINO2

The starting material, phenylboronic acid (76.84g, 630.2mmol) was dissolved in a THF (2780ml) in a round bottom flask, 4-bromo-1-iodo-2-nitrobenzene (309.96g, 945.3mmol), Pd (PPh 3 ) 4 (36.41g, 31.5mmol), K 2 CO 3 was (261.3g, 1890.6mmol), was added water (1390ml) and stirredat 80 . When the reaction is complete, CH 2 Cl 2 and the organic layer was extracted with water, MgSO 4 to the compound produced was dried andconcentrated to a silicagel column and the product was recrystallized 122.68g (yield: 70%) was obtained.

The synthetic route of 112671-42-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Duk San Neolux Co., Ltd.; Lee, Beom Song; Moon, Song Yun; Kim, Dae – Song; Park, Jong-chol; Lee, Gyu Min; Lee, Son-hee; (95 pag.)KR2015/87787; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 19821-80-8, A common heterocyclic compound, 19821-80-8, name is 1,3-Dibromo-2-iodobenzene, molecular formula is C6H3Br2I, 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.

Place 3-mercaptoindole (25g, 1eq), 1,3-dibromo-2-iodobenzene (60.62g, 1eq), cesium carbonate Cs2CO3(109.18g, 6eq)in a dry two-necked bottleWith a small amount of copper flakes (3.47g, 0.001eq), then add 250mL of dimethylformamide, warmed to 130 for 24 hours, the solvent was distilled off in vacuo, and then dichloromethane and water, the dichloromethane layer After drying with magnesium sulfate, spin-dry it, and then use silica gel column to separate and purify.The solid was obtained as an intermediate (Ir-072-a) with a yield of 83%.

The synthetic route of 19821-80-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangzhou Huarui Optoelectric Materials Co., Ltd.; Liang Zhiming; Yan Caijuan; Huang Hong; Pan Junyou; Chen Sihang; (52 pag.)CN111039987; (2020); A;,
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. 16355-92-3, name is 1,10-Diiododecane, A new synthetic method of this compound is introduced below., SDS of cas: 16355-92-3

Example 5 Preparation of 4,4′-(1,12-dodecanediyl)bispyridine LDA (2M) (20 mL, 40.00 mmol) was added dropwise to a solution of 4-picoline (3.73 g, 40.00 mmol) in THF (60 mL) at -78 C. The mixture was stirred for 30 min and then 1,10-diiododecane (6.31 g, 16.00 mmol) in THF (10 mL) was added dropwise. The resulting mixture was warmed to room temperature and stirred for 4 hrs. 50% saturated NH4Cl was added to the reaction mixture. The aqueous phase was extracted with ethylacetate (40 mL*2), and the combined organic liquors were washed with 50% saturated brine (40 mL*3) and saturated brine (40 mL), dried over anhydrous Na2SO4, and concentrated under reduced pressure. The crude product was purified by column chromatography (hexanes:ethylacetate 1:1 to 1:2) to afford 4.16 g of the title compound. Yield: 80%. 1H NMR (300 MHz, CDCl3) delta 1.18-1.40 (m, 16H), 1.53-1.70 (m, 4H), 2.59 (t, J=7.5 Hz, 4H), 7.10 (d, J=6.0 Hz, 4H), 8.48 (d, J=6.0 Hz, 4H) ppm; 13C NMR (75 MHz, CDCl3) delta 29.4, 29.7, 29.8, 29.9, 30.6, 35.5, 124.0, 149.6, 151.8 ppm.

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; Crooks, Peter; Dwoskin, Linda P.; Zheng, Guangrong; Sumithran, Sangeetha; US2009/318503; (2009); A1;,
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. 628-77-3, name is 1,5-Diiodopentane, A new synthetic method of this compound is introduced below., Quality Control of 1,5-Diiodopentane

To a solution of 31 (400mg, 1 .5 mmol) in anhydrous DMF (4 mL), in a flask purged with argon, was added K2C03 (320 mg, 1.5 mmol) and 1 ,5-diiodopentane 32 (1.1 mL, 7.6 mmol). The reaction mixture was heated to 60C until complete (30 minutes). The solution was diluted with CH2CI2 (50 mL) and washed with H20 (50 mL) and brine (50 mL) before the organics were dried with MgS04, filtered and the volatiles remove in vacuo. The crude material was purified by silica gel column chromatography (Hexane/EtOAc ; 100% to 3:7) to afford pure product 33 as a light brown foamy gum (61 1 mg, 87% yield). Analytical Data: RT 1 .51 min; MS (ES+) m/z (relative intensity) 458.95 ([M + H]+ , 100 ).

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; SPIROGEN SARL; HOWARD, Philip Wilson; WO2014/96365; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 628-77-3, 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. 628-77-3, name is 1,5-Diiodopentane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

1 ,5-diiodopentane (1 .54 mL, 3.35 g, 10.4 mmol) was added to a stirred solution of the phenol 12 (8.74 g, 20.7 mmol), TBAI (750 mg, 2.05 mmol) and K2003 (3.15 g, 22.8 mmol) in dry DMF (60 mL). The reaction mixture was heated to 70 00 and stirred under an argon atmosphere for 16 hours at which point analysis by LC/MS revealed substantial productformation at retention time 2.21 minutes, ES+ mlz 935 [M+ Na], 913 [M+ H]. The reaction mixture was allowed to cool to room temperature and the DMF was removed by evaporation in vacuo. The resulting residue was red issolved in EtOAc (200 mL) and the aqueous phase was washed with water (3 x 40 mL), brine (50 mL), dried (MgSO4), filtered and evaporated in vacuo to provide the crude product. Purification by lsoleraTM(Hexane/EtOAc, SNAP Ultra 100 g, 100 mL per minute) gave the bis-ether 13 (eluting at60% Hexane/EtOAc) as a yellow foam (6.75 g, 71% yield).

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, 1,5-Diiodopentane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MEDIMMUNE LIMITED; HOWARD, Philip Wilson; GREGSON, Stephen John; (228 pag.)WO2018/69490; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 21740-00-1, The chemical industry reduces the impact on the environment during synthesis 21740-00-1, name is 5-Bromo-2-iodobenzoic acid, I believe this compound will play a more active role in future production and life.

A solution of 5-bromo-2-iodobenzoic acid (10.0 g, 30.6 mmol) in DMF was treated with (2.11 g, 30.6 mmol) 1,2,3-triazole, 14.09 g (61.2 mmol) K3PO4.H2O and 583 mg (3.06 mmol) CuI. The mixture was heated at 60 C. for 3 hours with stirring under N2. The reaction was cooled to rt, diluted with water and acidified with 1N HCl. The mixture was partitioned with EtOAc three times. The organic layers were combined, rinsed with brine, dried over MgSO4, filtered and concentrated. The residue was purified by column chromatography (EtOAc in hexanes, 1% AcOH buffer) to give the faster eluting desired 5-bromo-2-(2H-1,2,3-triazol-2-yl)benzoic acid, A-3. Data for A-3: 1HNMR (500 MHz, DMSO-d6) delta 13.4 (br s, 1H), 8.12 (m, 2H), 7.94-7.88 (m, 2H), 7.78-7.73 (m, 1H) ppm. The undesired 5-bromo-2-(1H-1,2,3-triazol-2-yl)benzoic acid eluted second.

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, 5-Bromo-2-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Bergman, Jeffrey M.; Breslin, Michael J.; Coleman, Paul J.; Cox, Christopher D.; Mercer, Swati P.; Roecker, Anthony J.; US2008/132490; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com