HRID18684

反应详情

EQUATION

反应方程式

HRID 18684 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A solution of 23.07 g (100 mmol) of the hydrochloride of 2-butyl-1,3-diazaspiro[4,4]non-1-en-4-one and 19.8 g of potassium hydroxide in 100 mL de water is added to a solution of 29.7 g (100 mmol) of 4-iodobenzyl bromide and 3.4 g (10 mmol) of tetrabutylammonium bisulphate in 30 mL of toluene, and the mixture is heated at reflux for 1 hr. After cooling to 25° C., 100 mL of water is added and the phases are separated. To the organic phase is added 10 mL of concentrated hydrochloric acid, 100 mL is evaporated at reduced pressure, 300 mL of ethyl acetate is added and the resulting solid is filtered to give 39.6 g (88%) of the title compound in the form of hydrochloride.

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 1 hr
  3. customthe phases are separated
  4. additionTo the organic phase is added 10 mL of concentrated hydrochloric acid, 100 mL
  5. customis evaporated at reduced pressure, 300 mL of ethyl acetate
  6. additionis added
  7. filtrationthe resulting solid is filtered