反应详情

温度

40 °C

To 260 ml of ion-exchanged water were added 20 g of cyanocobalamin, 6.02 g of trimethylsulfonium iodide and 800 mg of iron(II) sulfate heptahydrate. The mixture was heated in a water bath and, after replacing the atmosphere of the system by nitrogen, a solution of sodium borohydride (8 g)/2N sodium hydroxide (0.2 ml)/water (40 ml) and 15 ml of 2-butanone were added dropwise thereto under stirring at an inner temperature of 40° C. over 20 minutes, respectively. After stirring for 15 minutes as it was, the mixture was cooled to 15° C. Further, 15 ml of 2-butanone was added thereto, followed by stirring overnight. The precipitates were collected by filtration and dried, to give 21.4 g of a crude product of the title compound. Thereto was added 200 ml of a 50% acetone aqueous solution, and the mixture was heated, adjusted to pH 6.5 with concentrated hydrochloric acid and then filtered. After washing with 40 ml of a 50% acetone aqueous solution, 630 ml of acetone was added dropwise to the filtrate, followed by stirring at 15° C. overnight. Precipitated crystals were collected by filtration and dried, to give 17 g of the title compound (yield 86%).

1. temperatureThe mixture was heated in a water bath
2. stirringAfter stirring for 15 minutes as it
3. temperaturethe mixture was cooled to 15° C
4. stirringby stirring overnight
5. filtrationThe precipitates were collected by filtration
6. customdried
7. customto give 21.4 g of a crude product of the title compound
8. temperaturethe mixture was heated
9. filtrationfiltered
10. washAfter washing with 40 ml of a 50% acetone aqueous solution, 630 ml of acetone
11. additionwas added dropwise to the filtrate
12. stirringby stirring at 15° C. overnight
13. customPrecipitated crystals
14. filtrationwere collected by filtration
15. customdried