HRID2288288
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
5.6 g of the product obtained in Stage 1 above is introduced into 8 ml of ammonium hydroxide, the mixture is taken to about -5° C. and 1.58 g of ammonium chloride and 1.23 g of sodium cyanide are added successively and the reaction medium is left to rise to ambient temperature for about 40 minutes then heated at 40° C.±5° C. under agitation overnight. It is returned to ambient temperature and extraction is carried out 3 times with chloroform, the organic phase is washed with salt water and dried. After purification on silica, eluting with cyclohexane-ethyl acetate: 3-7 with 0.5% of triethylamine, 4.41 g of expected product (pale yellow syrup) is obtained.
WORKUP
后处理
- customis taken to about -5° C.
- waitthe reaction medium is left
- temperaturethen heated at 40° C.±5° C. under agitation overnight
- customis returned to ambient temperature
- extractionextraction
- washthe organic phase is washed with salt water
- customdried
- customAfter purification on silica
- washeluting with cyclohexane-ethyl acetate