HRID728631
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
PROCEDURE
实验过程
A solution of 32.5 g (0.31 mole) of diethanolamine in 60 cm3 of pyridine are added slowly to a solution of 185 g (0.97 mole) of tosyl chloride in 220 cm3 of pyridine at 0° C. so that the temperature does not exceed 5° C. After the addition is complete, the mixture is maintained at this temperature for 1 h, then it is poured into 220 cm3 of ice-cold water with vigorous stirring. After filtration, washing and drying 148.4 g of precipitate are obtained (yield 85%; Rf=0.6 silica/CH2Cl2 /acetone/98/2).
WORKUP
后处理
- customdoes not exceed 5° C
- additionAfter the addition
- temperaturethe mixture is maintained at this temperature for 1 h
- filtrationAfter filtration
- washwashing
- dry with materialdrying 148.4 g of precipitate
- customare obtained (yield 85%; Rf=0.6 silica/CH2Cl2 /acetone/98/2)