Category: 56987-35-0

Adding a certain compound to certain chemical reactions, such as: 56987-35-0, name is 3,3-Dibromo-azepan-2-one, 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 56987-35-0, name: 3,3-Dibromo-azepan-2-one

11.3 g of the caprolactam was dissolved in 200 ml of methylene chloride,41.6 g of phosphorus pentachloride was added portionwise under ice-cooling, and the reaction was continued for 10 minutes after the completion of the addition. 1 g of zinc iodide was added under a nitrogen atmosphere,The reaction was allowed to proceed to room temperature for 1 hour. A solution of bromine in dichloromethane (32 g of bromine in 100 ml of dichloromethane) was then added dropwise,After completion of the addition, the mixture was stirred overnight. The ice bath was cooled to 0 to 5 degrees,The reaction was carefully poured into 500 ml of ice water,Extracted with dichloromethane for 5 times,Dried over anhydrous sodium sulfate,After concentration, a mixed solvent of petroleum ether and ethyl acetate was added,Precipitation of solid,Filtration gave 23 g of solid,Directly used in the next step reaction. 13.5 g of 3,3-dibromoheptalactam was dissolved in 70 ml of dry DMF,4 g of lithium chloride were added successively,7 grams of lithium carbonate,After heating to 130 C for 8 hours,DMF was distilled off,Purification by column afforded 7.1 g of a white solid,Yield 75%

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,3-Dibromo-azepan-2-one, and friends who are interested can also refer to it.

Reference:
Patent; Second Military Medical University,People’s Liberation Army; Miao, Zhen Yuan; Zhang, Wannian; Wu, yue Lin; Sheng, chun Quan; Zhuang, Chunlin; Xiao, Min; Yao, Jianzhong; Dong, Guoqiang; (40 pag.)CN105367495; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 56987-35-0, name is 3,3-Dibromo-azepan-2-one, 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. category: amides-buliding-blocks

A. 1-t-Butoxycarbonylmethyl-3,3-dibromoperhydroazepin-2-one To a suspension of 300 mg of sodium hydride in 25 ml THF add a solution of 2.71 g of 3,3-dibromoperhydroazepin-2-one [R. Wineman et al., J. Am. Chem. Soc., 80, 6233 (1958)] and 2.50 g of t-butyl iodoacetate in 25 ml THF, carrying out the operation under N2. Stir the reaction at room temperature for several hours, quench with aqueous NaHSO3, isolate the organic phase, dry and concentrate in vacuo to obtain 1-t-butoxycarbonylmethyl-3,3-dibromoperhydroazepin-2-one.

The synthetic route of 3,3-Dibromo-azepan-2-one has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Merck & Co., Inc.; US4409146; (1983); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 56987-35-0, name is 3,3-Dibromo-azepan-2-one, 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 56987-35-0, category: amides-buliding-blocks

11.3 g of the caprolactam was dissolved in 200 ml of methylene chloride,41.6 g of phosphorus pentachloride was added portionwise under ice-cooling, and the reaction was continued for 10 minutes after the completion of the addition. 1 g of zinc iodide was added under a nitrogen atmosphere,The reaction was allowed to proceed to room temperature for 1 hour. A solution of bromine in dichloromethane (32 g of bromine in 100 ml of dichloromethane) was then added dropwise,After completion of the addition, the mixture was stirred overnight. The ice bath was cooled to 0 to 5 degrees,The reaction was carefully poured into 500 ml of ice water,Extracted with dichloromethane for 5 times,Dried over anhydrous sodium sulfate,After concentration, a mixed solvent of petroleum ether and ethyl acetate was added,Precipitation of solid,Filtration gave 23 g of solid,Directly used in the next step reaction. 13.5 g of 3,3-dibromoheptalactam was dissolved in 70 ml of dry DMF,4 g of lithium chloride were added successively,7 grams of lithium carbonate,After heating to 130 C for 8 hours,DMF was distilled off,Purification by column afforded 7.1 g of a white solid,Yield 75%

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,3-Dibromo-azepan-2-one, and friends who are interested can also refer to it.

Reference:
Patent; Second Military Medical University,People’s Liberation Army; Miao, Zhen Yuan; Zhang, Wannian; Wu, yue Lin; Sheng, chun Quan; Zhuang, Chunlin; Xiao, Min; Yao, Jianzhong; Dong, Guoqiang; (40 pag.)CN105367495; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 56987-35-0, These common heterocyclic compound, 56987-35-0, name is 3,3-Dibromo-azepan-2-one, 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.

A solution of 3,3-dibromoazepan-2-one (15.7 g, 57.9 mmol) in piperidine (140 mL) was heated at reflux for 4.5 h under N2. The solution was then allowed to reach room temperature and washed with 0.50 M aq. NaHS03 (200 mL). The aqueous phase was extracted with CHC13 (3 x 100 mL) and the combined organic layers were washed with brine (1 x 300 mL), dried (MgS04) and concentrated to afford a brown, oily solid, that crystallized upon standing. The resulting solid was suspended in water, filtered, and washed with water and Et20 to give 1 (10.3 g, 91%) as a white solid: IR (ATR, neat) 3193, 2950, 2935, 2923, 2855, 1655, 1605 cm”1; 1H NMR (CDC13, 600 MHz) delta 6.51 (bs, 1 H), 5.06 (t, 1 H, J= 7.6 Hz), 3.22 (q, 2 H, J= 6.5 Hz), 2.78 (app t, 4 H, J= 5.3 Hz), 2.15 (q, 2 H, J= 7.2 Hz), 1.76 (app quint, 2 H, J= 6.8 Hz), 1.69-1.62 (m, 4 H), 1.54-1.48 (m, 2 H); 13C NMR (CDC13, 150 MHz) delta 171.5, 147.6, 105.4, 50.1, 39.5, 30.2, 25.5, 24.5, 21.5; HRMS (EI) m/z calcd for CiiH18N20 194.1419, found 194.1422.

Statistics shows that 3,3-Dibromo-azepan-2-one is playing an increasingly important role. we look forward to future research findings about 56987-35-0.

Reference:
Patent; UNIVERSITY OF PITTSBURGH – OF THE COMMONWEALTH SYSTEM OF HIGHER EDUCATION; WIPF, Peter; WANG, Qiming, Jan; WO2012/78859; (2012); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics