HRID728631

反应详情

EQUATION

反应方程式

HRID 728631 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customdoes not exceed 5° C
  2. additionAfter the addition
  3. temperaturethe mixture is maintained at this temperature for 1 h
  4. filtrationAfter filtration
  5. washwashing
  6. dry with materialdrying 148.4 g of precipitate
  7. customare obtained (yield 85%; Rf=0.6 silica/CH2Cl2 /acetone/98/2)