HRID1579773

反应详情

EQUATION

反应方程式

HRID 1579773 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 11.97 g of 3-(3'-chloro-2'-hydroxypropyl)-benzhydrol, 120 ml of ethanol, 2.4 ml of water and 2.66 g of potassium cyanide was refluxed for 3 hours and then evaporated to dryness. The residue was taken up in 200 ml of methylene chloride and the organic phase was washed with water, dried over sodium sulfate, treated with activated carbon, filtered and evaporated to dryness. The residue was chromatographed over silica and was eluted with a 75-25 methylene chloride-ethyl acetate mixture which was evaporated to obtain 7.8 g of 3-(3'-cyano-2'-hydroxypropyl)-benzhydrol in the form of an orange amorphous solid soluble in chloroform and insoluble in water.

WORKUP

后处理

  1. temperaturewas refluxed for 3 hours
  2. customevaporated to dryness
  3. washthe organic phase was washed with water
  4. dry with materialdried over sodium sulfate
  5. additiontreated with activated carbon
  6. filtrationfiltered
  7. customevaporated to dryness
  8. customThe residue was chromatographed over silica
  9. washwas eluted with a 75-25 methylene chloride-ethyl acetate mixture which
  10. customwas evaporated