HRID2288288

反应详情

EQUATION

反应方程式

HRID 2288288 的结构方程式

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

  1. customis taken to about -5° C.
  2. waitthe reaction medium is left
  3. temperaturethen heated at 40° C.±5° C. under agitation overnight
  4. customis returned to ambient temperature
  5. extractionextraction
  6. washthe organic phase is washed with salt water
  7. customdried
  8. customAfter purification on silica
  9. washeluting with cyclohexane-ethyl acetate