At the same time, in my other blogs, there are other synthetic methods of this type of compound, Benzyl (2-bromoethyl)carbamate, and friends who are interested can also refer to it.
Adding a certain compound to certain chemical reactions, such as: 53844-02-3, name is Benzyl (2-bromoethyl)carbamate, 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 53844-02-3, HPLC of Formula: C10H12BrNO2
1.7 g of 5-hydroxy-2-nitrophenyl ethanol and 4.3 g of potassium carbonate were dispersed in 20 ml N, N’- dimethyl formamide, and heated to 60 deg.] C for 1 hour. It was slowly added dropwise 2.82 g N- benzyloxycarbonyl-BrEA in methylene chloride (5 ml), 60 reaction for 24 hours. After completion of the reaction, the solvent was removed under reduced pressure, the product was dissolved in ethyl acetate, washed with saturated sodium bicarbonate solution, and saturated sodium chloride solution each, washed twice with distilled water wash, the organic phase was dried over anhydrous magnesium sulfate and 8 hours, filtered after concentration under reduced pressure, ethyl acetate / cyclohexane recrystallized twice to give product A.Take 1.56 g of product A was dissolved in 50 ml of anhydrous dichloromethane, was added under ice-cooling 1.25 g N- benzyloxycarbonyl-methionine, 1.33 g N, N’- dicyclohexyl carbodiimide and 0.2 g 4 – dimethylaminopyridine, stirred at room temperature overnight. After completion of the reaction, diluted hydrochloric acid with ice, saturated sodium bicarbonate solution and saturated sodium chloride solution each, washed twice with distilled water wash, dried over anhydrous sodium sulfate overnight. Suction filtered and the solvent was removed under reduced pressure, recrystallized twice from ethyl acetate. The obtained crystals were dissolved in 20 ml of chloroform, 20 ml of hydrogen chloride in ethyl acetate under ice-cooling a saturated solution, after 6 hours at room temperature the reaction dried under reduced pressure to give the productB. The product B was dissolved 0.687 g of methylene chloride and 50 ml of a mixed solvent of 8 ml of pyridine, cooled to -18 deg.] C, was added dropwise 10 ml of a toluene solution of phosgene (1.93 mol per liter) for 6 hours. The reaction mixture was washed with dilute hydrochloric acid each and twice with saturated sodium bicarbonate solution, saturated sodium chloride solution and distilled water for each wash. The organic phase was dried overnight over anhydrous magnesium sulfate, concentrated under reduced pressure after filtration
At the same time, in my other blogs, there are other synthetic methods of this type of compound, Benzyl (2-bromoethyl)carbamate, and friends who are interested can also refer to it.
Reference:
Patent; Sichuan University; Ding, Mingming; Wang, Rui; Wu, Qiang; Tan, Hong; Zhang, Qin; Li, Jiehua; (14 pag.)CN105601550; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics