HRID263084

反应详情

EQUATION

反应方程式

HRID 263084 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 13 g (0.0365 mol) of the mesylate of Example 34 and of 32.5 g (0.365 mol) of 2-amino-2-methyl-1-propanol is heated slowly to 170° C. The reaction mixture is allowed to return to ambient temperature and is taken up in water. The insoluble matter is extracted with diethyl ether and the organic phase obtained is washed with water and dried over dry sodium sulphate to give, after evaporation of the solvent, 12.7 g of a limpid pale yellow oil. After treating 12 g of this oil in a solution of hydrogen chloride in diethyl ether, and purifying the product by crystallisation from ethyl acetate, 11.2 g of a white powder which is soluble in water to the extent of 200 g/l are obtained.

WORKUP

后处理

  1. customto return to ambient temperature
  2. extractionThe insoluble matter is extracted with diethyl ether
  3. customthe organic phase obtained
  4. washis washed with water
  5. dry with materialdried over dry sodium sulphate
  6. customto give
  7. customafter evaporation of the solvent, 12.7 g of a limpid pale yellow oil
  8. additionAfter treating 12 g of this oil in a solution of hydrogen chloride in diethyl ether
  9. custompurifying the product
  10. customby crystallisation from ethyl acetate, 11.2 g of a white powder which
  11. customare obtained