HRID444101
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 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
- temperaturemaintained gentle refluxing
- filtrationthe product was filtered off
- washwashed with water
- dry with materialdried over magnesium sulphate
- filtrationfiltered
- customThe solvent was removed
- customto give a brown oil which
- customslowly crystallised
- customRecrystallisation from petroleum ether