HRID444101

反应详情

EQUATION

反应方程式

HRID 444101 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of the product of stage (c) (183 g) in ethanol (150 ml) was heated to reflux. A solution of sodium cyanide (25 g) in hot water (50 ml) was added which maintained gentle refluxing. The mixture was then stirred for 5 minutes, poured into ice water, and the product was filtered off, taken up in dichloromethane, washed with water, dried over magnesium sulphate and filtered. The solvent was removed to give a brown oil which slowly crystallised. Recrystallisation from petroleum ether gave the title product as colourless needles, mp 87°-88° C.

WORKUP

后处理

  1. temperaturemaintained gentle refluxing
  2. filtrationthe product was filtered off
  3. washwashed with water
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. customThe solvent was removed
  7. customto give a brown oil which
  8. customslowly crystallised
  9. customRecrystallisation from petroleum ether