HRID978706
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionAfter addition
- stirringthe mixture was stirred for 2.5 hours at 135° C
- temperatureAfter cooling
- extractionthe solution was extracted with pentane
- washThe extract was washed with water
- stirringshaken with 5% (w/w) sulfuric acid in order
- extractionto extract the basic 3,3-bis(hydroxymethyl)-1-benzylazetidine acetone acetal