Category: 749927-69-3

Electric Literature of 749927-69-3, 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 749927-69-3 as follows.

A 200 liter reactor was charged with 4-bromo-2-fluoro-N-methylbenzamide (12.0 kg, 51.7 mole)1-Aminocyclobutane carboxylic acid(6.3 kg, 61.7 mole),Potassium carbonate (16.5 kg, 155 mole),2-acetylcyclohexanone (0.12 kg, 1.05 mole),1.2 liters of water, dissolved in 70 liters of DMF, under stirring with stirring CuI (0.2kg, 1.05mol)Heated to 110 degrees, the reaction 24 hours. After the reaction was completed, add water cooling 120 liters,Then add ethyl acetate extraction.The aqueous phase was retained, adjusted to pH = 1 with 1 N hydrochloric acid and the precipitated solid was filtered. Beating with water,Get pure 11.8 kg, product 86%.

According to the analysis of related databases, 749927-69-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shanghai Xipu Pharmaceutical Technology Co., Ltd.; Lianyungang Shengfeng Chemical Co., Ltd.; Qin Yong; Chen Yue; Bian Junjie; Yu Jianhua; Wang Mingfa; Dai Xiaoming; (6 pag.)CN107501237; (2017); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 749927-69-3, name is 4-Bromo-2-fluoro-N-methylbenzamide, belongs to amides-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 749927-69-3, COA of Formula: C8H7BrFNO

A) 2-fluoro-N-methyl-4-vinylbenzamide A mixture of 4-bromo-2-fluoro-N-methylbenzamide (0.80 g) , vinylboronic acid pinacol cyclic ester (0.80 g) and 2M aqueous sodium carbonate solution (3.45 mL) in DME (17.3 mL) was argon- purged. Bis (triphenylphosphine)palladium(II) dichloride (0.12 g) was added thereto, and the mixture was stirred overnight at 80C. The reaction solution was diluted with ethyl acetate, and the mixture was washed with water and saturated brine. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was subjected to short silica gel column chromatography, and the solvent was evaporated under reduced pressure to give the title compound (0.74 g) . MS: [M+H]+ 180.1.

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, 4-Bromo-2-fluoro-N-methylbenzamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; YAMADA, Masami; SUZUKI, Shinkichi; SUGIMOTO, Takahiro; NAKAMURA, Minoru; SAKAMOTO, Hiroki; KAMATA, Makoto; WO2015/163485; (2015); A1;,
Amide – Wikipedia,
Amide – 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 749927-69-3 as follows. COA of Formula: C8H7BrFNO

A mixture of 4-bromo-2-fluoro-N-methylbenzamide (900 mg, 3.9 mmol), 5-(4,4,5,5- tetramethyl-l,3,2-dioxaborolan-2-yl)pyrimidin-2-amine (710 mg, 3.2 mmol), tetrakis(triphenylphosphine)palladium (100 mg, 0.1 mmol) and potassium carbonate (1.3 g, 9.7 mmol) in toluene (6.0 mL) and ethanol (3.0 mL) and water (3.0 mL) was heated at 110 0C for 2 hours. After cooling to RT, the reaction mixture was quenched with water and extracted with diethyl ether. The solid was filtered and washed with water and diethyl ether to afford the desired product (720 mg).

According to the analysis of related databases, 749927-69-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; INCYTE CORPORATION; ZHUO, Jincong; METCALF, Brian; WO2008/64157; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 749927-69-3, name is 4-Bromo-2-fluoro-N-methylbenzamide, molecular formula is C8H7BrFNO, 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. Recommanded Product: 4-Bromo-2-fluoro-N-methylbenzamide

To a stirred solution of 4-bromo-2-fluoro-N-methylbenzamide (6.4 g, 27.5 mmol), 1-aminocyclopropanecarboxylic acid (4.29 g, 42.4 mmol), CuI (1.047 g, 5.5 mmol), K2CO3 (9.50 g, 68.0 mmol), in DMF (64 mL) was added H2O (6.4 mL), triethylamine (0.164 mL, 1.1 mmol) followed by 2-acetyl cyclohexanone (0.717 g, 5.10 mmol). The reaction mixture was stirred at 100 C. overnight. The reaction was monitored by TLC and LCMS. H2O was added, and the aqueous layer was washed with ethyl acetate. The aqueous layer was acidified with 1M citric acid solution (pH?4) and extracted with ethyl acetate. The organic extracts were dried over anhydrous Na2SO4, concentrated under reduced pressure and crystallized with DCM to afford 3.01 g of the title compound as an off-white solid

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 749927-69-3, its application will become more common.

Reference:
Patent; MEDIVATION TECHNOLOGIES, INC.; Chakravarty, Sarvajit; Jain, Rajendra Parasmal; US2013/79372; (2013); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 749927-69-3, 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. 749927-69-3, name is 4-Bromo-2-fluoro-N-methylbenzamide, This compound has unique chemical properties. The synthetic route is as follows.

100 ml of DMF was added to a 250 ml three-necked flask,A solution of 18.5 g of 5,5-dimethyl-3- (3-trifluoromethyl-4-fluorophenyl) -2-thiamidazol-4-one was successively added with stirring,Ice bath cooling to 0-5 C,Add 3.9 g of sodium hydride in portions.Plus,The ice bath continues to stir for 30 min.13.68 g of 2-fluoro-4-bromobenzoylmethylamine was dissolved in 30 ml of DMF,Slowly add it toIn the reaction solution, control the internal temperature 0-5 C.Plus finished, returned to room temperature, continue to stir 5h,TLC monitoring reaction is completed.The reaction solution was addedTo 500 ml of water, filtered to obtain crude.After drying, column chromatography was performed to obtain 23.9 g of enterine, the yield was 87.3%.

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

Reference:
Patent; Chengdu Yinuo Dabo Pharmaceutical Technology Co., Ltd.; Fu Qingquan; Yue Lijian; Lin Qiang; Liao Xianbo; Zhao Maoxian; Qin Yan; (8 pag.)CN104844520; (2017); B;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 749927-69-3, 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 749927-69-3 as follows.

A 200 liter reactor was charged with 4-bromo-2-fluoro-N-methylbenzamide (12.0 kg, 51.7 mole)1-Aminocyclobutane carboxylic acid(6.3 kg, 61.7 mole),Potassium carbonate (16.5 kg, 155 mole),2-acetylcyclohexanone (0.12 kg, 1.05 mole),1.2 liters of water, dissolved in 70 liters of DMF, under stirring with stirring CuI (0.2kg, 1.05mol)Heated to 110 degrees, the reaction 24 hours. After the reaction was completed, add water cooling 120 liters,Then add ethyl acetate extraction.The aqueous phase was retained, adjusted to pH = 1 with 1 N hydrochloric acid and the precipitated solid was filtered. Beating with water,Get pure 11.8 kg, product 86%.

According to the analysis of related databases, 749927-69-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shanghai Xipu Pharmaceutical Technology Co., Ltd.; Lianyungang Shengfeng Chemical Co., Ltd.; Qin Yong; Chen Yue; Bian Junjie; Yu Jianhua; Wang Mingfa; Dai Xiaoming; (6 pag.)CN107501237; (2017); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 749927-69-3,Some common heterocyclic compound, 749927-69-3, name is 4-Bromo-2-fluoro-N-methylbenzamide, molecular formula is C8H7BrFNO, 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.

4-bromo-2-fluoro -N- methylbenzamide, 2-amino – isobutyric acid molar ratio, catalyst, co-catalyst, acid binding agent, followed by water 1:1.5:0.1:0.1:4:2.3 In a single-neck flask was added4-bromo-2-fluoro -N- methylbenzamide (10g, 43.1mmol), 2- amino – isobutyric acid (6.7g, 64.7mmol), potassium carbonate (23.8g, 172.4mmol), proline (0.7g, 4.31mmol), water (1.8ml, 100mmol) was dissolved in DMF (60ml), andStirring under nitrogen replacementAfter addition of CuCl (0.45g, 4.31mmol), was heated to 100 , reaction 24h.After completion of the reaction first added water (120ml) the mixture was diluted, added and extracted with dichloromethane, the organic phase was removed, the aqueous phase was adjusted pH = 4 with 1mol / L citric acid solution, and the precipitated solid was filtered. The solid washed with water and ethanol (100: 1) mixed solution was washed three times to give pure white solid 9.5g. Yield 87%

The synthetic route of 749927-69-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ferguson (Wuhan) Biotechnology Co., Ltd.; Su, Ji; Ouyang, Kangle; Fu, Qiang; Lu, Wei; (5 pag.)CN105330560; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 749927-69-3, The chemical industry reduces the impact on the environment during synthesis 749927-69-3, name is 4-Bromo-2-fluoro-N-methylbenzamide, I believe this compound will play a more active role in future production and life.

N-methyl-2-fluoro-4-bromo-benzamide 1a (23.21 g, 100 mmol) was added to a three-necked flask.Cyclobutyrate hydrochloride 2 (15.16 100 mmol) and N,N-dimethylacetamide (116 mL),Copper iodide (1.90 g, 10 mmol) and cesium carbonate (71.68 g, 220 mmol) were added under a nitrogen atmosphere, and the mixture was stirred and heated to 90 to 95 C overnight.At the end of the reaction, water (232 mL) and isopropyl acetate (232 mL) were added, and the mixture was stirred and the aqueous phase was collected, and the pH was adjusted to 3 to 4 with 4N hydrochloric acid.Precipitating a large amount of solids,Filtration dried to give compound 3 (17.88 g, 79%).

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, 4-Bromo-2-fluoro-N-methylbenzamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hangzhou Kechao Biological Technology Co., Ltd.; Zheng Xuchun; Zhang Yiping; (10 pag.)CN108383749; (2018); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 749927-69-3, These common heterocyclic compound, 749927-69-3, name is 4-Bromo-2-fluoro-N-methylbenzamide, 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 stirred suspension of zinc powder (2.5 g, 38.5 mmol) in anhydrous N,N-d m ethyl form a ide (10 mL) under nitrogen was added iodine (200 mg). After 5 min, a solution of methyl (f?)-2-((/er/-butoxycarbonyl)amino)-3-iodopropanoate (5.0 g, 15.2 mmol) in A( A’-di m ethyl form a i de (10 mL) was added slowly over lOmin. The mixture was stirred at rt for 30min. A suspension of 4-bromo-2-fluoro-Af- methylbenzamide (2.8 g, 12 mmol), Pd2(dba)3 (280 mg, 0.3 mmol), and 2- dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (Sphos, 250 mg, 0.6 mmol) in /V,/V- dimethylformamide (10 mL) was added into the zinc reagent mixture. The reaction mixture was heated at 50C and stirred overnight. After cooling, the reaction mixture was quenched with water, diluted with EtOAc and filtered through Celite. The filter cake was washed with EtOAc and the filtrate was washed with brine, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by flash column chromatography over silica gel (0-80% EtO Ac/hexane) to afford the desired product as a beige solid (4.0 g, 94%). LC-MS: 377.1 [M+Na]+; 1H NMR (400MHz, CDCl3) d 8.04 (t, 1H, J = 8.1 Hz), 7.02 (d, 1H, J = 8.0 Hz), 6.91 (d, 1H, J = 12.8 Hz), 6.70 (m, 1H), 5.02 (d, 1H, J = 8.0 Hz), 4.60 (m, 1H), 3.73 (s, 3H), 3.18 (dd, 1H, J = 13.8, 5.4 Hz), 3.07 (m, 1H), 3.03 (d, 3H, J = 4.6 Hz), 1.43 (s, 9H).

The synthetic route of 749927-69-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EPIODYNE, INC.; MEDINA, Julio Cesar; MCGEE, Larry; WEI, Zhi-Liang; SADLOWSKI, Corinne; SEIDL, Frederick; BHATT, Ulhas; WANG, Xiaodong; NGUYEN, Thomas; SPERANDIO, David; DING, Pingyu; NERURKAR, Alok; LI, Yihong; DUQUETTE, Jason; (307 pag.)WO2019/195634; (2019); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

749927-69-3, Adding a certain compound to certain chemical reactions, such as: 749927-69-3, name is 4-Bromo-2-fluoro-N-methylbenzamide, belongs to amides-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 749927-69-3.

100 ml of DMF was added to a 250 ml three-necked flask,A solution of 18.5 g of 5,5-dimethyl-3- (3-trifluoromethyl-4-fluorophenyl) -2-thiamidazol-4-one was successively added with stirring,Ice bath cooling to 0-5 C,Add 3.9 g of sodium hydride in portions.Plus,The ice bath continues to stir for 30 min.13.68 g of 2-fluoro-4-bromobenzoylmethylamine was dissolved in 30 ml of DMF,Slowly add it toIn the reaction solution, control the internal temperature 0-5 C.Plus finished, returned to room temperature, continue to stir 5h,TLC monitoring reaction is completed.The reaction solution was addedTo 500 ml of water, filtered to obtain crude.After drying, column chromatography was performed to obtain 23.9 g of enterine, the yield was 87.3%.

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, 4-Bromo-2-fluoro-N-methylbenzamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Chengdu Yinuo Dabo Pharmaceutical Technology Co., Ltd.; Fu Qingquan; Yue Lijian; Lin Qiang; Liao Xianbo; Zhao Maoxian; Qin Yan; (8 pag.)CN104844520; (2017); B;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics