HRID978706

反应详情

EQUATION

反应方程式

HRID 978706 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
135 °C

PROCEDURE

实验过程

A mixture of 30.2 g of 5,5-bis(bromomethyl)-2,2-dimethyl-1,3-dioxane (0.1 mol), 24.0 g of sodium bicarbonate and 50 ml of dimethyl sulfoxide was heated to 135° C. A solution of 10.7 g of benzylamine in 50 ml of DMSO was then added dropwise with stirring over 1.5 hours. After addition was complete, the mixture was stirred for 2.5 hours at 135° C. After cooling, 100 ml of DMSO and 20 ml of water were added and the solution was extracted with pentane. The extract was washed with water and then shaken with 5% (w/w) sulfuric acid in order to extract the basic 3,3-bis(hydroxymethyl)-1-benzylazetidine acetone acetal.

WORKUP

后处理

  1. additionAfter addition
  2. stirringthe mixture was stirred for 2.5 hours at 135° C
  3. temperatureAfter cooling
  4. extractionthe solution was extracted with pentane
  5. washThe extract was washed with water
  6. stirringshaken with 5% (w/w) sulfuric acid in order
  7. extractionto extract the basic 3,3-bis(hydroxymethyl)-1-benzylazetidine acetone acetal