HRID1081536

反应详情

EQUATION

反应方程式

HRID 1081536 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

In a reactor, 117 g (0.6 mol) of N-methyl-D-glucamine were dissolved in a mixture of 800 ml of water and 400 ml of tetrahydrofuran, and 201.6 g (2.4 mol) of sodium hydrogen carbonate were then dispersed. While the temperature of the reaction mixture was maintained at 5° C., 115.6 g (0.6 mol) of 2-ethylhexyl chloroformate were added dropwise, and the mixture was then allowed to react for 3 hours with stirring at 5° C. and left standing overnight at room temperature. The reaction mixture was then filtered and concentrated; the pasty residue obtained was dissolved in 2 liters of acetone and then filtered after cooling to 5° C. The crystallized product collected was dried. 105 g (50% yield) of N-(2-ethylhexyloxycarbonyl)-N-methyl-D-glucamine, the melting point of which is 74° C., were obtained.

WORKUP

后处理

  1. additionwere then dispersed
  2. customto react for 3 hours
  3. waitleft
  4. filtrationThe reaction mixture was then filtered
  5. concentrationconcentrated
  6. customthe pasty residue obtained
  7. filtrationfiltered
  8. temperatureafter cooling to 5° C
  9. customThe crystallized product collected
  10. customwas dried