Реакция #1061323

Уравнение реакции

D-glucosamine hydrochloride

sodium hydrogen carbonate

trichloroethoxycarbonyl chloride

→

N-trichloroethoxycarbonyl-D-glucosamine

Растворители

water

Условия реакции

Обработка

1. 1
   Температураby cooling in an ice bath
2. 2
   Температураcooling for 2 hours
3. 3
   ФильтрацияThe precipitate was collected by filtration
4. 4
   Промывкаwashed successively with water and diethyl ether
5. 5
   Другоеrecrystallized from 95% ethanol

Методика

Thirty grams of D-glucosamine hydrochloride was dissolved in 500 ml of water, and 30.0 g of sodium hydrogen carbonate was added thereto, followed by cooling in an ice bath. To the cooled solution was added 27.5 ml of trichloroethoxycarbonyl chloride, and the mixture was stirred under ice-cooling for 2 hours and then at room temperature for 11 hours. The precipitate was collected by filtration, washed successively with water and diethyl ether, and recrystallized from 95% ethanol to obtain 42.3 g of N-trichloroethoxycarbonyl-D-glucosamine (Compound A) having a melting point of 183° to 184° C. (with decomposition).

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