Month: February 2021

Reference of 10061-02-6, 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. 10061-02-6 name is trans-1,3-Dichloropropene, 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.

A mixture of step (2) obtained N- hydroxy phthalimide was dissolved in 10%aqueous sodium hydroxide was added dropwise at room temperature 65.8g of trans-1,3-D, the reaction is complete, filtration to give 2-(3-chloro-allyloxy)isoindole-1,3-dione

At the same time, in my other blogs, there are other synthetic methods of this type of compound, trans-1,3-Dichloropropene, and friends who are interested can also refer to it.

Reference:
Patent; Shandong Kaisheng New Materials Co., Ltd.; Wang, Deyao; Zhang, Taiming; Wu, Yixia; Wu, Qiang; Song, Liwei; Xie, Shengming; (5 pag.)CN105348139; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 50594-82-6, 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. 50594-82-6, name is 3,4,5-Trichlorobenzotrifluoride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 3; Preparation method of 3,4,5-trifluorobenzotrifluoride; 860 g of dry sulpholane and 524 g of dry KF were initially charged with exclusion of moisture in an autoclave, and 500 g of 3,4,5-trichlorobenzotrifluoride, 5 g of nitrobenzene and 25 g of CNC catalyst were added. The vessel was sealed and the mixture subsequently heated to 200 C. for 5 h and then to 220 C. for a further 12 h. During the reaction, a maximum total pressure of 9 bar arose. The mixture was then cooled to 20 C. and decompressed into a cooled receiver. The product was distilled off at standard pressure. After redistillation of the crude product, 300 g of 3,4,5-trifluorobenzotrifluoride (75% of theory) were obtained as a colourless liquid.

The synthetic route of 3,4,5-Trichlorobenzotrifluoride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Pleschke, Axel; Marhold, Albrecht; US2006/9643; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 873-38-1, 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. 873-38-1, name is 2-Bromo-4-chloroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In a 20 mL microwave vial was added 2-bromo-4-chloroaniline (3 g, 14.53 mmol), 4,4,5, 5-tetramethyl-2-(tetramethyl-l,3,2-dioxaborolan-2-yl)-l,3,2-dioxaborolane (5.53 g, 21.80 mmol), KOAc (3.66 g, 37.3 mmol), Pd(dppf)Cl2-CH2Cl2adduct (0.32 g, 0.44 mmol) and DMSO (9 mL). The resulting suspension was purged with N2, capped and heated at 80 C for 22 h. The reaction was cooled to rt. Water was added to dissolve the salts, then the reaction was filtered. The remaining solid was suspended in DCM and the insoluble solid was filtered. The filtrate was concentrated and then purified by normal phasechromatography to give 4-chloro-2-(tetramethyl-l ,3,2-dioxaborolan- 2-yl)aniline (3.15 g, 86 % yield) as a white solid. MS (ESI) m/z: 172.3 (M-CeHio+H)+. NMR (400MHz, CDCh) delta 7.54 (d, J=2.6 Hz, IH), 7.13 (dd, J=8.8, 2.6 Hz, IH), 6.52 (d, J=8.6 Hz, IH), 4.72 (br. s., 2H), 1.34 (s, 12H).

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-Bromo-4-chloroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; ZHU, Yeheng; DILGER, Andrew K.; EWING, William R.; ORWAT, Michael J.; PINTO, Donald J.P.; (156 pag.)WO2017/19821; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 20816-79-9, 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. 20816-79-9, name is 1-Bromo-8-chloronaphthalene, This compound has unique chemical properties. The synthetic route is as follows.

Under a nitrogen atmosphere,the intermediate A-BE, 1-bromo-8-chloronaphthalene, and potassium carbonate were mixed at a molar ratio of 1: (1.0-1.2):3.0 under a nitrogen atmosphere, and added to the catalyst containing palladium acetate and tri-tert-butylphosphine tetrafluoroboratein toluene/water,Under reflux with nitrogen for 12-16h, cooled down, the reaction solution is allowed to stand for liquid separation, dried, and purified by column chromatography to obtain intermediate M-1.

The chemical industry reduces the impact on the environment during synthesis 1-Bromo-8-chloronaphthalene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; CECEP Wanrun Co., Ltd.; Li Qing; Li Zishu; Shi Yu; Meng Fanmin; Zhou Yinbo; Hu Baohua; (17 pag.)CN108586319; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 203302-92-5, name is 3-Bromo-2-chloro-6-fluorotoluene, A new synthetic method of this compound is introduced below., SDS of cas: 203302-92-5

N-bromosuccinimide (“NBS”) (6.42 g) and benzoyl peroxide (catalytic amount) in carbon tetrachloride (40 ml) was heated to reflux. A 500 watt tungsten halogen lamp was used to initiate the reaction. The reaction mixture was heated to reflux and irradiated for 30 minutes. The reaction mixture was allowed to cool to ambient temperature and then filtered. The filtrate was concentrated to give a colorless oil which solidified on standing to give l-bromo-3-bromomethyl-2-chloro-4-fluoro-benzene as an off-white solid (10.7 g). IH-NMR (400 MHz, CDCl3): 7.58 (dd, IH), 6.94 (t, IH), 4.64 (d, 2H) 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; SYNGENTA LIMITED; WO2009/63180; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 1716-42-3, These common heterocyclic compound, 1716-42-3, name is 1-(3-Chloropropoxy)-4-fluorobenzene, 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.

EXAMPLE 40 A mixture of 6.5 parts of 1-[(4-fluorophenyl)methyl]-2-(4-piperidinylmethyl)-1H-benzimidazole, 4.2 parts of sodium carbonate and 120 parts of 4-methyl-2-pentanone was stirred and refluxed for 30 minutes using a water separator. 5.2 Parts of 1-(3-chloropropoxy)-4-fluorobenzene were added at reflux temperature and stirring was continued for 3 hours at this temperature using a water separator. After cooling to room temperature, the salts were filtered off and the filtrate was washed twice with water, dried, filtered and evaporated. The residue was converted into the ethanedioate salt in 2-propanone. The salt was filtered off, washed with 2-propanone and crystallized from methanol. The product was filtered off and dried in vacuo at 80¡ã C., yielding 7 parts (53percent) of 2-[[1-[3-(4-fluorophenoxy)propyl]-4-piperidinyl]methyl]-1-[(4-fluorophenyl)methyl]-1H-benzimidazole ethanedioate (1:2); mp. 186.7¡ã C. (119).

Statistics shows that 1-(3-Chloropropoxy)-4-fluorobenzene is playing an increasingly important role. we look forward to future research findings about 1716-42-3.

Reference:
Patent; Janssen Pharmaceutica, N.V.; US4695575; (1987); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 38762-41-3, name is 4-Bromo-2-chloroaniline, 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 38762-41-3, HPLC of Formula: C6H5BrClN

To a stirred solution of 4-bromo-2-chloroaniline (1.8 g, 8.82 mmol) in dry THF (20 mL) was added NaHMDS (11.5 mL 69.68 mmol) followed by Etl (0.9 ml, 2.95 mmol) at RT. The reaction mixture was stirred at RT for lh. The reaction mixture was quenched with aqueous NH4Cl solution and extracted with EtOAc (2X50 mL), dried over Na2S04 and concentrated under reduced pressure to afford the title compound (1.5 g,75%), LCMS: m/z = 264.0[M+2]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-2-chloroaniline, and friends who are interested can also refer to it.

Reference:
Patent; AURIGENE DISCOVERY TECHNOLOGIES LIMITED; CHIKKANNA, Dinesh; KHAIRNAR, Vinayak V.; RAMACHANDRA, Muralidhara; SATYAM, Leena Khare; (139 pag.)WO2019/142126; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 6579-54-0 as follows. Product Details of 6579-54-0

C. 3-(2,6-dichlorophenylsulfonylamino)-4-(2-pyridyl)-5-(3-(4-fluorophenoxy)benzylthio)-(1H)-pyrazole 3-Amino-4-(2-pyridyl)-5-(3-(4-fluorophenoxy)benzylthio)-(1H)-pyrazole (0.39 g, 0.99 mmol) was dissolved in 5 ml of pyridine. Commercial 2,6-dichlorobenzenesulfonyl chloride (0.26 g, 1.04 mmol) was added and the red solution was stirred overnight at room temperature. The reaction mixture was poured into 50 ml of water and was extracted twice with 100 ml portions of ethyl acetate. The organic layers were washed with water and brine, combined, dried over MgSO4 and concentrated. The crude product was slurried in cold ethyl acetate and the solid was filtered off and washed with small portions of cold ethyl acetate and cold diethyl ether and dried under vacuum to afford 0.32 g (53% yield) of the final compound. FD-MS: (M+)600 mp. 164-5 C. Elemental analysis: Calc. C 53.91% H 3.18% N 9.31% S 10.66% Cl 11.79% Found C 54.19% H 3.20% N 9.37% S 9.80% Cl 11.79%

According to the analysis of related databases, 6579-54-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Eli Lilly and Company; US5972972; (1999); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 363-51-9, 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. 363-51-9, name is 2-Chloro-6-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows.

To a stirred solution of 4-bromo-2-butoxy-5-fluorobenzoic acid (Intermediate 2, 1.36 g, 4.67 mmol) and catalyticDMF in anhydrous DCM (25 mL) was added oxalyl chloride (490 ml, 5.6 mmol) dropwise. The resulting mixture wasstirred for 1 h and concentrated under reduced pressure. A solution of the residue in anhydrous DCM (20 mL) was addeddropwise to a stirred solution of 2-chloro-6-fluoroaniline (750 mg, 5.15 mmol) and triethylamine (720 ml, 5.2 mmol) inanhydrous DCM (30 mL). Following complete addition, the mixture stirred for 1 h. The mixture was concentrated underreduced pressure. The residue was dissolved in ethanol (15 mL) and precipitated by slow addition of water (30 mL).The solid was collected on a filter, washed with water and dried in a vacuum oven to yield 1.73 g (88 % yield) of thedesired product.LC-MS: Rt = 1.55 min; MS (ESIpos): m/z = 418 [M+H]+1H-NMR (400 MHz, DMSO-d6) delta [ppm]: 0.787 (0.48), 0.889 (6.64), 0.908 (16.00), 0.926 (7.83), 1.390 (0.52), 1.408(1.83), 1.427 (3.10), 1.446 (3.07), 1.464 (1.83), 1.483 (0.50), 1.731 (0.76), 1.747 (2.12), 1.767 (2.57), 1.784 (2.05), 1.801(0.67), 2.518 (3.81), 2.523 (2.64), 4.165 (2.33), 4.181 (4.62), 4.197 (2.31), 7.329 (0.79), 7.348 (1.90), 7.367 (1.26), 7.372(1.43), 7.380 (1.00), 7.395 (0.95), 7.400 (1.79), 7.414 (1.86), 7.421 (1.38), 7.433 (4.14), 7.438 (3.57), 7.453 (1.07), 7.458(0.93), 7.579 (2.69), 7.593 (2.74), 7.612 (3.05), 7.634 (2.88), 9.836 (4.40).

The chemical industry reduces the impact on the environment during synthesis 2-Chloro-6-fluoroaniline. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Bayer AG; Gradl, Stefan, Nikolaus; Niehues, Michael; Halfbrodt, Wolfgang; (43 pag.)EP3553052; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 2533-69-9,Some common heterocyclic compound, 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, molecular formula is C3H4Cl3NO, 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 1 N-(3-indolylmethyl)-trichloroacetamidine A solution of 5.72 g. (0.033 mole) of methyl trichloroacetimidate in 15 ml. of benzene is added over 15 minutes to a stirred solution of 3.18 g. (0.022 mole) of 3-aminomethylindole in 25 ml. dry dimethylsulfoxide at room temperature. The mixture is stirred for 20 hours at room temperature, concentrated to dryness, and the residue taken up in warm chloroform. The chloroform solution is washed with 2 portions of water and extracted with 3 portions of dilute hydrochloric acid. The aqueous acid extracts are combined, extracted with 2 portions of chloroform and filtered. The clear aqueous filtrate is made basic with a saturated aqueous solution of sodium bicarbonate and the product extracted into 3 portions of chloroform. The combined chloroform extracts are washed with water, dried over magnesium sulfate, filtered and concentrated to dryness to afford N-(3-indolylmethyl)-trichloroacetamidine, which after crystallization from benzene/hexane has a m.p. of 135.5 to 138.5 C.

The synthetic route of 2533-69-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Merck & Co., Inc.; US4065465; (1977); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics