反应详情

5.6 g of the product of Stage 1 were introduced into 8 ml of ammonium hydroxide and the mixture was brought to about -5° C. 1.58 g of ammonium chloride and 1.23 g of sodium cyanide were added successively and the mixture was allowed to return to ambient temperature for about 40 minutes, then heated to 40° C.±5° C. with stirring overnight. The reaction medium was returned to ambient temperature and extraction was carried out 3 times with chloroform. The organic phase was washed with salt water and dried. After purification on silica with ethyl cycloacetate/triethylamine; 3/7 as eluant, 4.41 g of the expected product (pale yellow syrup) were obtained.

1. customwas brought to about -5° C
2. temperatureheated to 40° C.±5° C.
3. customwas returned to ambient temperature
4. extractionextraction
5. washThe organic phase was washed with salt water
6. customdried
7. customAfter purification on silica with ethyl cycloacetate/triethylamine