HRID1763264

反应详情

EQUATION

反应方程式

HRID 1763264 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

16 ml (0.22 mol) of liquid phosgene are condensed into 33 g (0.15 mol) of 2,2-dibromopropanol in 150 ml of CH2Cl2, at -20° C, and 12 ml (0.15 mol) of pyridine in 15 ml of CH2Cl2 are then added slowly dropwise at -20° C to -5° C and the mixture is stirred for a further 2 hours at 20° C. The solution is washed, at 0° C, with water, 5% strength sulphuric acid and H2O and dried (Na2SO4) and the solvent is stripped off (46.1 g of crude product). Vacuum distillation gives 36.3 g (86%) of 2,2-dibromopropoxycarbonyl chloride as a colorless liquid. Boiling point12 = 81°-86° C.

WORKUP

后处理

  1. washThe solution is washed, at 0° C, with water, 5% strength sulphuric acid and H2O
  2. dry with materialdried (Na2SO4)
  3. distillationVacuum distillation