反応 #1061323

反応方程式

D-glucosamine hydrochloride

sodium hydrogen carbonate

trichloroethoxycarbonyl chloride

→

N-trichloroethoxycarbonyl-D-glucosamine

溶媒

water

反応条件

後処理

1. 1
   温度by cooling in an ice bath
2. 2
   温度cooling for 2 hours
3. 3
   ろ過The precipitate was collected by filtration
4. 4
   洗浄washed successively with water and diethyl ether
5. 5
   その他recrystallized from 95% ethanol

実験手順

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).

出典