HRID1250431

反应详情

EQUATION

反应方程式

HRID 1250431 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

Ethylamine (42 ml of a 70% solution in water, 530 mmol) is added slowly to a stirred mixture of isophorone (9.67 g, 70 mmol) and ethylamine hydrochloride (0.29 g, 3.5 mmol) at -7° C. After the addition is complete, the temperature of the mixture is allowed to rise to room temperature, and the mixture is stirred for a further 72 hours. The mixture is subsequently cooled to 10° C., and potassium hydroxide (44.9 g, 800 mmol) is added in portions. After 45 minutes, ice is added and the mixture is stirred. The organic phase is then separated, dried over sodium sulfate and evaporated in vacuo to give the crude product (11.0 g, 95%) as a yellow oil, which is used immediately without further purification in the following step.

WORKUP

后处理

  1. additionAfter the addition
  2. customto rise to room temperature
  3. waitAfter 45 minutes
  4. additionice is added
  5. stirringthe mixture is stirred
  6. customThe organic phase is then separated
  7. dry with materialdried over sodium sulfate
  8. customevaporated in vacuo