2613-32-3 Archives - Chlorides-buliding-blocks

18-Sep-2021 News Continuously updated synthesis method about 2613-32-3

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2613-32-3, its application will become more common.

Some common heterocyclic compound, 2613-32-3, name is 2-Chloro-4,5-difluoroaniline, molecular formula is C6H4ClF2N, 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. SDS of cas: 2613-32-3

Lithium 1,1,1,3,3,3-hexamethyldisilazan-2-ide (42 ml, 1 M solution in tetrahydrofuran, 42 mmol, CAS No 4039-32-1 ) was added drop wise within 5 minutes to a solution of 2-chloro-4,5-difluoroaniline (3.88 g, 23.2 mmol) in tetrahydrofuran (1 10 ml) at -78 C and the mixture was stirred for 1 h at that temperature. A solution of ethyl 4-{[tert-butyl(diphenyl)silyl]oxy}-1-(2-chloroethyl)cyclohexanecarboxylate (10.0 g, 21 .1 mmol) in tetrahydrofuran (1 10 ml) was added and the mixture was stirred for 2 h at -78(C. The mix ture was warmed to room temperature and stirred for 4 d. For work-up, the reaction mixture was added to a mixture of water and sodium bicarbonate solution and the mixture was extracted with ethyl acetate (3x). The combined organic phases were washed with sodium chloride, dried over sodium sulfate and concentrated under reduced pressure, the residue was purified by flash chromatography (340 g Snap cartridge, hexane/ethyl acetate gradient, 5% -> 25% ethyl acetate). The product containing fractions were concentrated and were purified a second time by flash chromatography (120 g Snap cartridge, hexane/ethyl acetate gradient, 5% -> 25% ethyl acetate) to give the title compound in 2 fractions: fraction 1 (7.53 g, single isomer based on1H NMR, isomer 1, contains impurities from aniline and isomer 2), fraction 2 (1 .13 g, isomer 2). Fraction 1 (isomer 1 ):1H-NMR (400 MHz, DMSO-d6): delta [ppm] = 7.67-7.55 (m, 5H), 7.52-7.30 (m, 9H), 3.97 (br s, 1H), 3.60 (t, 2H), 2.15-2.07 (m, 2H), 2.04 (t, 2H), 1 .76-1 .63 (m, 2H), 1 .58-1 .45 (m, 2H), 1 .39-1 .27 (m, 2H), 1 .05 (s, 9H). LC-MS (Method 1 ): Rt= 1 .80 min; MS (ESIpos): m/z 518.3 [M+H]+

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2613-32-3, its application will become more common.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; BUCHGRABER, Philipp; EIS, Knut; WAGNER, Sarah; SUeLZLE, Detlev; VON NUSSBAUM, Franz; BENDER, Eckhard; LI, Volkhart, Min-Jian; LIU, Ningshu; SIEGEL, Franziska; LIENAU, Philipp; (248 pag.)WO2018/78005; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Introduction of a new synthetic route about 2613-32-3

The synthetic route of 2-Chloro-4,5-difluoroaniline has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 2613-32-3, name is 2-Chloro-4,5-difluoroaniline, 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. name: 2-Chloro-4,5-difluoroaniline

1-Chlor-1-dimethylamino-2-methyl-1-propen (64.9 mg, 0.486 mmol) was added to a solution of trans-4-[(pyrazolo[1 ,5-a]pyrim idin-3-ylcarbonyl)am ino]cyclohexanecarboxylic acid (70.0 mg, 0.243 mmol) in dichloromethane (3.1 ml) and the mixture was stirred at roomtemperature for 30 mi Pyridine (59 p1, 0.0.73 mmol) and 2-chloro-4,5-difluoroaniline (39.7 mg, 0.243 mmol, GAS No 261 3-32-3) were added and the mixture was stirred over night at room temperature. For work-up, water was added and the reaction mixture was extracted with dichloromethane. Die organic phase was filtrated through a silicone filter, concentrated and the residue purified by preparative HPLG (Method 9) to yield the title compound (3.8 mg,4% yield).LG-MS (Method 2): R = 1 .10 mm; MS (ESIpos) m/z = 434.1 [M+H].1HNMR (400 MHz, DMSO-d6): 6 [ppm] = 9.62 (5, 1H), 9.32 (dd, 1H), 8.83 (dd, 1H), 8.58 (5,1H), 7.86-7.76 (m, 3H), 7.28 (dd, 1H), 3.90-3.76 (m, 1H), 2.12-1.91 (m, 4H), 1.66-1.50 (m,2H), 1.45-1.31 (m, 2H).

The synthetic route of 2-Chloro-4,5-difluoroaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; EIS, Knut; ACKERMANN, Jens; WAGNER, Sarah; BUCHGRABER, Philipp; SUeLZLE, Detlev; HOLTON, Simon; BENDER, Eckhard; LI, Volkhart; LIU, Ningshu; SIEGEL, Franziska; LIENAU, Philip; BAIRLEIN, Michaela; VON NUSSBAUM, Franz; HERBERT,Simon; KOPPITZ, Marcus; (734 pag.)WO2016/177658; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Brief introduction of 2-Chloro-4,5-difluoroaniline

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-4,5-difluoroaniline, its application will become more common.

Electric Literature of 2613-32-3,Some common heterocyclic compound, 2613-32-3, name is 2-Chloro-4,5-difluoroaniline, molecular formula is C6H4ClF2N, 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.

To a suspension of 100 mg (0.28 mmol) trans-4-({[4-(phenoxycarbonyl)-1H-imidazol-5-yl]carbonyl}amino)cyclohexane-carboxylic acid in 5 ml dichloromethane 62 p1(0.45 mmol) 1-chloro-N,N,2-trimethylprop-1-en-1-amine were added and the mixture was stirred at roomtemperature for 30 minutes. 68 p1(0.84 mmol) pyridine and 31 p1(0.28 mmol) 2-chloro-4,5-difluoroaniline were added and the reaction was stirred at room temperature for 30 minutes.

Continuously updated synthesis method about C6H4ClF2N

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2613-32-3, its application will become more common.

Introduction of a new synthetic route about 2613-32-3

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-4,5-difluoroaniline, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 2613-32-3, name is 2-Chloro-4,5-difluoroaniline, belongs to chlorides-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 2613-32-3, Product Details of 2613-32-3

1-Chloro-4,5-difluoro-2-isothiocyanatobenzene To a mixture of 2-chloro-4,5-difluoroaniline (1 equiv.) and sodium hydroxide (3 equiv.) in DCM (0.24 M) and water (0.24 M) was added dropwise thiophosgene (3 equiv.) at 0 C. The reaction mixture was stirred at 25 C. overnight. TLC showed the reaction was complete. The organic phase was separated and dried over MgSO4, then concentrated to give 1-chloro-4,5-difluoro-2-isothiocyanatobenzene (53%) as a white solid.

Reference:
Patent; Signal Pharmaceuticals, LLC; Alexander, Matthew; Bahmanyar, Sogole; Hansen, Joshua; Huang, Dehua; Hubbard, Robert; Jeffy, Brandon; Leisten, Jim; Moghaddam, Mehran; Raheja, Raj K.; Raymon, Heather; Schwarz, Kimberly; Sloss, Marianne; Torres, Eduardo; Tran, Tam Minh; Xu, Shuichan; Zhao, JingJing; Boylan, John Frederick; (317 pag.)US2016/96841; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Analyzing the synthesis route of 2613-32-3

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 2613-32-3.

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. 2613-32-3, name is 2-Chloro-4,5-difluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 2-Chloro-4,5-difluoroaniline

[ithium 1,1,1 ,3,3,3-hexamethyldisilazan-2-ide (42 ml, 1 M solution in tetrahydrofuran, 42 mmol, CAS No 4039-32-1) was added drop wise within 5 minutes to a solution of 2-chloro- 4,5-difluoroaniline (3.88 g, 23.2 mmol) in tetrahydrofuran (110 ml) at -780 and the mixture was stirred for 1 h at that temperature. A solution of ethyl 4-{[tert-butyl(diphenyl)silyl]oxy}-1 – (2-chloroethyl)cyclohexanecarboxylate (10.0 g, 21.1 mmol) in tetrahydrofuran (110 ml) wasadded and the mixture was stirred for 2 h at -78G. The mixture was warmed to room temperature and stirred for 4 d. For work-up, the reaction mixture was added to a mixture of water and sodium bicarbonate solution and the mixture was extracted with ethyl acetate (3x). The combined organic phases were washed with sodium chloride, dried over sodium sulfate and concentrated under reduced pressure, the residue was purified by flash chromatography (340 g Snap cartridge, hexane/ethyl acetate gradient, 5% -> 25% ethyl acetate). The productcontaining fractions were concentrated and were purified a second time by flash chromatography (120 g Snap cartridge, hexane/ethyl acetate gradient, 5% -> 25% ethyl acetate) to give the title compound in 2 fractions: fraction 1 (7.53 g, single isomer based on 1H NMR, isomer 1, contains impurities from aniline and isomer 2), fraction 2(1.13 g, isomer2).Fraction 1 (isomer 1): 1H-NMR (400 MHz, DMSO-d6): 6 [ppm] = 7.67-7.55 (m, 5H), 7.52-7.30 (m, 9H), 3.97 (brs, 1H), 3.60 (t, 2H), 2.15-2.07 (m, 2H), 2.04 (t, 2H), 1.76-1.63 (m, 2H), 1.58- 1.45 (m, 2H), 1.39-1.27 (m, 2H), 1.05 (5, 9H).[C-MS (Method 1): R = 1.80 mm; MS (ESIpos): m/z = 518.3 [M¡ÂH]

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 2613-32-3.

Application of 2613-32-3

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.

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. 2613-32-3, name is 2-Chloro-4,5-difluoroaniline, A new synthetic method of this compound is introduced below., category: chlorides-buliding-blocks

General procedure: Different substituted anilines 3 (10.0mmol) were added to a solution of hydrochloric acid (15mL, 3-4mol L-1), and then sodium nitrite (0.76g, 10.5mmol) dissolving in water (3mL) was dropwise added at 0C. After 0.5h, tin (II) chloride (4.5g, 20mmol) in 10mL of concentrated hydrochloric acid was dropwise added to the above mixture. The reaction was vigorously stirred for 2h at 0C, and then was filtered and washed with 3-4molL-1 hydrochloric acid. The precipitate was dissolved in water and filtered. The filtrate was adjusted to pH 12, and the generated solid was collected and dried to afford different substituted phenylhydrazine 4a-k.

Reference:
Article; Liu, Jing-Bo; Li, Feng-Yun; Dong, Jing-Yue; Li, Yu-Xin; Zhang, Xiu-Lan; Wang, Yuan-Hong; Xiong, Li-Xia; Li, Zheng-Ming; Bioorganic and Medicinal Chemistry; vol. 26; 12; (2018); p. 3541 – 3550;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics