反应详情

温度

35 °C

To 130 ml of ion-exchanged water were added 10 g of cyanocobalamin, 2.85 g of trimethylsulfoxonium chloride, 700 mg of iron (II) sulfate heptahydrate and 7.5 ml of 2-butanone. After replacing the atmosphere of the system by nitrogen, the mixture was heated in a water bath. A solution of sodium borohydride (4 g)/2N sodium hydroxide (0.5 ml)/water (20 ml) was added dropwise thereto under stirring at an inner temperature of 35° C. After stirring for 3 hours as it was, the mixture was cooled to 15° C. and then stirred overnight. Thereto was added 7.5 ml of butanone, followed by stirring for 2 hours. Then, the precipitates were collected by filtration and dried, to give 35 g of a crude product of the title compound. Thereto was added 140 ml of a 50% acetone aqueous solution. The mixture was heated at 45° C., filtered and washed with 60 ml of a 50% acetone aqueous solution. After the mixture was adjusted to pH 6.5 with concentrated hydrochloric acid, 475 ml of acetone was added dropwise thereto and the mixture was stirred at 20° C. overnight. Precipitated crystals were collected by filtration and dried, to give 8.92 g of the title compound (yield 89.9%).

1. temperaturethe mixture was heated in a water bath
2. stirringAfter stirring for 3 hours as it
3. temperaturethe mixture was cooled to 15° C.
4. stirringstirred overnight
5. stirringby stirring for 2 hours
6. filtrationThen, the precipitates were collected by filtration
7. customdried
8. customto give 35 g of a crude product of the title compound
9. temperatureThe mixture was heated at 45° C.
10. filtrationfiltered
11. washwashed with 60 ml of a 50% acetone aqueous solution
12. additionwas added dropwise
13. stirringthe mixture was stirred at 20° C. overnight
14. customPrecipitated crystals
15. filtrationwere collected by filtration
16. customdried