Continuously updated synthesis method about 1871-57-4

The chemical industry reduces the impact on the environment during synthesis 1871-57-4. I believe this compound will play a more active role in future production and life.

The chemical industry reduces the impact on the environment during synthesis 1871-57-4, name is 3-Chloro-2-chloromethyl-1-propene, I believe this compound will play a more active role in future production and life. 1871-57-4

Part 2; A mixture of (2S)-benzylamino-succinic acid 1-benzyl ester 4-tert-butyl ester (12.1 g, 32.6 mmol), K2CO3 (14 g, 3 equiv.), NaI (3.0 g, 20 mmol) and 1-chloro-2-chloromethyl-1- propene (5.1 g, 40.8 mmol) in MeCN (150 mL) was stirred at 81C for 16 h. After cooling, the reaction mixture was filtered and the filtrate was concentrated under reduced pressure. Purification by Combiflash (hexane and ethyl acetate: gradient 0 to 8% during 12 min) afforded (2S)- [benzyl- (2-chloromethyl-allyl)-amino]-succinic acid 1-benzyl ester 4-tert-butyl ester (8.7 g, 58%). MS (ESI): 458 (M + H+).

The chemical industry reduces the impact on the environment during synthesis 1871-57-4. I believe this compound will play a more active role in future production and life.

Reference:
Patent; INCYTE CORPORATION; WO2005/37826; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

The important role of 5-Chloro-1H-benzo[d][1,2,3]triazole

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-Chloro-1H-benzo[d][1,2,3]triazole, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 94-97-3, name is 5-Chloro-1H-benzo[d][1,2,3]triazole, 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 94-97-3, 94-97-3

General procedure: 1-phenylbutane-1,3-dione 1a (0.2 mmol, 32.4 mg), 1H-benzo[d][1,2,3]triazole 2a (0.2 mmol, 23.8 mg), N-bromosuccinimide (NBS) (39.2 mg, 1.2 equiv), KOtBu (44.8 mg, 2 equiv) and EtOAc (2 mL) were added to a flask with a magnetic stirring bar. The resulting mixture was stirred for 6 h at 60 oC. After cooling to room temperature, the mixture was diluted with ethyl acetate and filtered. The filtrate was removed under reduced pressure to get the crude product, which was further purified by silica gel chromatography (petroleum/ethyl acetate = 5/1-2/1 as eluent) to give product 3a and 4a as light yellow and pink solids. The identity and purity of the products was confirmed by 1H and 13C NMR spectroscopic analysis

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-Chloro-1H-benzo[d][1,2,3]triazole, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Chen, Wen-Lin; Li, Ji-Hui; Meng, Xu; Tang, Dong; Guo, Shuai-Bo; Chen, Bao-Hua; Tetrahedron Letters; vol. 54; 4; (2013); p. 295 – 299;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Simple exploration of 2,6-Dichlorobenzenesulfonyl chloride

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. 6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride, A new synthetic method of this compound is introduced below., 6579-54-0

2,6-Dichloro-3-nitrobenzenesulfonic acid Lithium hydroxide hydrate (12.64 g, 0.301 mol) was added to a solution of 2,6-dichlorobenzenesulfonyl chloride (35.53 g, 0.146 mol) in MeOH (600 mL) and the reaction was allowed to stir at room temperature for 3 hr. The reaction mixture was filtered to remove suspended solids and then concentrated. The resulting solid was dried in vacuo overnight to remove any residual MeOH. The solid was then dissolved in H2SO4 (300 mL) and chilled in an ice bath. A solution of H2S04 (35 mL) and HNO3 (13.2 mL) was slowly added to the above reaction over 90 min. The reaction was allowed to warm up to room temperature overnight and then slowly poured into ice water (1200 mL) and extracted with EtOAc. The combined organic layers were dried (MgSO4) and concentrated to yield 2,6-dichloro-3-nitrobenzenesulfonic acid (44.35 g, 99%) as the dihydrate. EI-MS (m/z) 270 (M-H)-.

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; SmithKline Beecham Corporation; US6500863; (2002); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some tips on 772-49-6

The synthetic route of 772-49-6 has been constantly updated, and we look forward to future research findings.

772-49-6, A common heterocyclic compound, 772-49-6, name is 1-Chloro-3-(trifluoromethoxy)benzene, molecular formula is C7H4ClF3O, 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.

To a cooed (-.78 C) souUon of 1-choro-3-(trfluoromethoxy)benzene (20 g, 102 mrno)n THF (100 mL) was added n-butyWthum (2.5 M/hexanes, 41 mL, 102 mmo) dropwseover a period of 10 minutes. Strrng was mantaned at -78C for I h, and then asouDon of odne (26 g, 102 rnrno) n THF (100 mL) was added dropwse at -.78 C overa perod of 30 ninutes. After the add Won, the temperature was niantaned at -78 C for1 h and then aflowed to warm to rt and stirred for a tota of 18 h. The reacton mixturewas poured nto saturated aqueous Na2SO3 and extracted wfth EtOAc (2 x 200 mL). The combined organc extracts were dried over Na2SO4 and concentrated n vacuo to give the tWe compound as an oH (28 g, 85% yed). 1H NMR (500 MHz, CDC3) oe 7.40 (dd, J = 81, 1.4 Hz, IH), 7.32 (t, J = 8.1 Hz, IH), 7.16 (dt, J = 8.2, 1.4 Hz, IH).

The synthetic route of 772-49-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; AMERIKS, Michael K.; RAVULA, Suchitra; SAVALL, Bradley M.; SWANSON, Devin M.; ZIFF, Jeannie M.; SHIREMAN, Brock T.; (167 pag.)WO2016/176463; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Introduction of a new synthetic route about 41965-95-1

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 41965-95-1.

41965-95-1, Adding some certain compound to certain chemical reactions, such as: 41965-95-1, name is 3-Chloro-4-methoxybenzylamine Hydrochloride, 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 41965-95-1.

(1) A mixture of 3-methylthio-5-hydroxy-6-ethoxycarbonyl-1,2,4-triazine (see Chem. Ber., 2179-2184, 97 (1964)) 546 mg and thionyl chloride 10 ml is stirred at 60-70 C. for 5 hours. The mixture is concentrated in vacuo, and to the residue is added 3-chloro-4-methoxybenzylamine hydrochloride 634 mg and dimethylformamide 20 ml, and further triethylamine 770 mg in dimethylformamide 20 ml. After stirring for 3 hours at room temperature, the mixture is poured into water and extracted with ethyl acetate. The combined ethyl acetate layer is washed with water and brine, concentrated in vacuo. The residue is purified with silica gel chromatography (solvent; chloroform_methanol=50:1) to give 3-methylthio-5-(3-chloro-4-methoxybenzylamino)-6-ethoxycarbonyl-1,2,4-triazine as a pale yellow solid, 769 mg. mp 101-105 C. MS(m/z): 369(M+H)+

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 41965-95-1.

Reference:
Patent; Yamada, Koichiro; Matsuki, Kenji; Omori, Kenji; Kikkawa, Kohei; US2004/142930; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Analyzing the synthesis route of 13078-79-0

The synthetic route of 2-(3-Chlorophenyl)ethanamine has been constantly updated, and we look forward to future research findings.

A common heterocyclic compound, 13078-79-0, name is 2-(3-Chlorophenyl)ethanamine, molecular formula is C8H10ClN, 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. 13078-79-0.

General procedure: Compound 3 (0.37 g, 1 mmol), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide (EDC, 0.29 g,1.5 mmol), 1-hydroxybenzotrizole (HOBT, 0.20 g, 1.5 mmol) and CHCl3 (20 mL) were stirred at roomtemperature for 1 h, and then different amines (3 mmol) were added. The solution was stirred atroom temperature overnight. Then the solvent was poured into water and extracted with ethylacetate (20 mL ¡Á 3). The solution was dried over anhydrous Na2SO4 and concentrated. The residues were purified by flash chromatography with chloroform/petroleum ether (2:1, v/v) elution.

The synthetic route of 2-(3-Chlorophenyl)ethanamine has been constantly updated, and we look forward to future research findings.

Reference:
Article; Li, Bo; Huang, Ai-Ling; Zhang, Yi-Long; Li, Zeng; Ding, Hai-Wen; Huang, Cheng; Meng, Xiao-Ming; Li, Jun; Molecules; vol. 22; 7; (2017);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Extracurricular laboratory: Synthetic route of 6940-78-9

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, 6940-78-9, other downstream synthetic routes, hurry up and to see.

A common compound: 6940-78-9, name is 1-Bromo-4-chlorobutane, belongs to chlorides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 6940-78-9

After 7-hydroxy-lH-quinolin-2-one (10 g) and DMF (50 ml) were heated to approximately 30C, an aqueous potassium carbonate solution (potassium carbonate: 8.6 g, water: 10 ml) was added. After the mixture was stirred at 30 to 40C for about 15 minutes, l-bromo-4-chlorobutane (14.3 ml) was added and stirred at approximately 40C for 5 hours. Water (100 ml) was added dropwise over a period of 30 minutes or more while the temperature was maintained at 30C or more. After the mixture was stirred at approximately 30C for 30 minutes, stirring was continued at 10C or less for 1 hour, after which the precipitated crystals were collected by filtration. After methanol (100 ml) was added to the precipitated crystals, the mixture was stirred under reflux to ensure dissolution. This solution was cooled and stirred at 30 to 40C for 30 minutes and then at 5C or less for about 1 hour, after which the precipitated crystals were collected by filtration. The crystals were dried at 60C to obtain 7- (4-chlorobutoxy) -lH-quinolin-2-one as white powder. Yield: 12.3 g ^I-NMR (300 MHz; CDC13) oppm; 1.95-2.05 (4H, m) , 3.64 (2H, t, J = 6.0Hz), 4.10 (2H, t. J = 5.5 Hz), 6.56 (1H, d, J = 9.5 Hz), 6.80 (1H. dd, J = 9.0 Hz, 2.5 Hz), 6.84 (1H, d, J = 2.5 Hz), 7.45 (1H, d, J = 9.0 Hz), 7.73 (1H, d, J = 9.5 Hz), 12.45 (1H, brs).

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, 6940-78-9, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; OTSUKA PHARMACEUTICAL CO., LTD.; SHINHAMA, Koichi; UTSUMI, Naoto; SOTA, Masahiro; FUJIEDA, Shigeo; OGASAWARA, Shin; WO2013/15456; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

The important role of 7781-10-4

The synthetic route of 7781-10-4 has been constantly updated, and we look forward to future research findings.

7781-10-4, 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. 7781-10-4, name is 4-Chloro-7-methyl-7H-pyrrolo[2,3-d]pyrimidine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Add N-bromosuccinimide (418 g, 2.35 mol) portionwise over 20 min at 15 C to a solution of 4-chloro-7-methyl-pyrrolo[2,3-d]pyrimidine (355 g, 2.12 mol) indichloromethane (3.19 L), and stir at 23 C for 3 h. After this time, filter, wash with H20 (5.32 L), and dry to give the title compound (448 g, 86%) as a white solid. ES/MS m/z (35C1,79Br) 245.9 (M+H).

The synthetic route of 7781-10-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; CIFUENTES-GARCIA, Marta Maria; GARCIA-PAREDES, Maria Cristina; (34 pag.)WO2018/194885; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Simple exploration of 3-Chloro-4-methoxybenzylamine Hydrochloride

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. 41965-95-1, name is 3-Chloro-4-methoxybenzylamine Hydrochloride, A new synthetic method of this compound is introduced below., 41965-95-1

9-[(3-chloro-4-methoxybenzyl)amino]-2-ethyl-7-(trifluoromethyl)-2,3-dihydro-lH- pyrrolo[3,4-b]quinolin-l-one M [00304] A solution of 49 (0.095 mmol), 3-chloro-4-methoxybenzylamine hydrochloride (0.14 mmol) and (‘pr)2NEt (0.57 mmol) in n-propanol (1.0 mL) was heated to 90 C for lh. The solvent was evaporated off and the residue was purified by flash chromatography (AcOEt) to give the final product M. MS ESI (m/z) 450 (M+H)+; 1H NMR (400 MHz, CDC13) delta 8.58 (t, IH, J=6.0 Hz), 8.46 (s, IH), 8.0 (d, IH, J=8.8 Hz), 7.80 (dd, IH, Ji=2.0, J2=9.2 Hz), 7.45 (d, IH, J=2.0 Hz), 7.32 (dd, IH, Ji=2.4, J2=8.4 Hz), 6.95 (d, IH, J=8.0 Hz), 4.95 (d, 2H, J=6.0 Hz), 4.41 (s, 2H), 3.90 (s, 3H), 3.67 (q, 2H, J=7.2 Hz), 1.3 (t, 3H, J=7.2 Hz)

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 TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK; LANDRY, Donald, W.; DENG, Shixian; FIORITO, Jole; ARANCIO, Ottavio; WASMUTH, Andrew; WO2015/9930; (2015); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Simple exploration of 1996-29-8

The chemical industry reduces the impact on the environment during synthesis 1-Bromo-4-chloro-2-fluorobenzene. I believe this compound will play a more active role in future production and life.

1996-29-8, The chemical industry reduces the impact on the environment during synthesis 1996-29-8, name is 1-Bromo-4-chloro-2-fluorobenzene, I believe this compound will play a more active role in future production and life.

Step 1 : To a lOOmL three-necked flask was added 20mL toluene and compound 13a (3g, 0.014mol, l .Oeq), compound 13b (4.3g, 0.022mol, 1.5eq) and t-BuONa (2.064g, 0.022mol, 1.5eq). The reaction was heated to 80oC with nitrogen. Then BINAP (0.3g, 0.42mmol, 0.03eq) and Pd2(dba)3.CHCl3 (0.15g, 0.14mmol, O.OOleq) was added to the stirred mixture . The reaction was heated to reflux for 18h. The solution was cooled, concentrated and extracted with 30 EA from lOmL water. The organic layer was washed with brine , dried , concentrated in vacuum and purified by column chromatography on silica gel eluted with PE: EA= 10: 1 to afford the compound 13c (4g, HPLC: 98%) as a white solid. Yield: 86%.

The chemical industry reduces the impact on the environment during synthesis 1-Bromo-4-chloro-2-fluorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; LIANG, Congxin; (62 pag.)WO2018/5713; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics