HRID328342

反应详情

EQUATION

反应方程式

HRID 328342 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20.4 G. (0.2 moles) of 3-hexanol is added dropwise under anhydrous conditions to 345 ml. (0.4 moles) of 12.5% phosgene in benzene with stirring and cooling in an ice bath. The addition is complete in 2 hours and 15 minutes and the temperature is allowed to warm to room temperature and the reaction mixture is stirred overnight. Gaseous nitrogen is passed through the solution for several hours to remove the excess phosgene and hydrogen chloride. The reaction mixture is then evaporated to dryness in vacuo affording 28.3 g. (86%) of a colorless oil which infrared analysis indicates to have a strong carbonyl band and no hydroxy band. The oil is used as is in subsequent reactions.

WORKUP

后处理

  1. temperaturecooling in an ice bath
  2. additionThe addition
  3. waitGaseous nitrogen is passed through the solution for several hours
  4. customto remove the excess phosgene and hydrogen chloride
  5. customThe reaction mixture is then evaporated to dryness in vacuo
  6. customaffording 28.3 g