反应详情

温度

40 °C

To 1.3 l of ion-exchanged water were added 100 g of cyanocobalamin and 32.46 g of trimethylsulfoxonium iodide, 4 g of iron(II) sulfate heptahydrate and 100 ml of 2-butanone. Under a nitrogen stream, the mixture was heated in a water bath and a solution of sodium borohydride (40 g)/2N sodium hydroxide (1 ml)/water (200 ml) was added dropwise thereto under stirring at an inner temperature of 40° C. over 30 minutes. After stirring for 30 minutes as it was, the mixture was returned to room temperature and further stirred overnight. The precipitates were collected by filtration and dried, to give 123 g of a crude product of the title compound. Thereto was added 1 l of a 50% acetone aqueous solution, and the mixture was heated at 35° C., adjusted to pH 7.0 with concentrated hydrochloric acid and then filtered. 2.8 l of acetone was added dropwise thereto, followed by stirring overnight. Precipitated crystals were collected by filtration and dried, to give 93.2 g of the title compound (yield 94%).

1. temperatureUnder a nitrogen stream, the mixture was heated in a water bath
2. stirringAfter stirring for 30 minutes as it
3. waitthe mixture was returned to room temperature and further stirred overnight
4. filtrationThe precipitates were collected by filtration
5. customdried
6. customto give 123 g of a crude product of the title compound
7. temperaturethe mixture was heated at 35° C.
8. filtrationfiltered
9. addition2.8 l of acetone was added dropwise
10. stirringby stirring overnight
11. customPrecipitated crystals
12. filtrationwere collected by filtration
13. customdried