反应详情

温度

2.5 °C

6-(5-Chloropyridin-2-yl)-5,7-dioxo-5,6-dihydropyrrolo-[3,4-b]-pyrazine (100g) was suspended in 900 ml water. The slurry was cooled to 0-5° C. and 100 ml (7.2%) of aqueous sodium borohydride solution stabilized with 0.1 g sodium hydroxide was added in 3 hrs under vigorous stirring. Reaction mixture was stirred at 0-5° C. for 4 to 5 hrs. After completion of reaction solid was filtered and washed with 2×300 ml water. The filtered solid was refluxed in 215 ml dichloromethane for 30 min and cooled to 25-30° C. The solid was filtered, washed with 100 ml dichloromethane and dried at 50-60° C. to obtain 82 g of title compound.

1. additionwas added in 3 hrs under vigorous stirring
2. customReaction mixture
3. customAfter completion of reaction solid
4. filtrationwas filtered
5. washwashed with 2×300 ml water
6. temperatureThe filtered solid was refluxed in 215 ml dichloromethane for 30 min
7. temperaturecooled to 25-30° C
8. filtrationThe solid was filtered
9. washwashed with 100 ml dichloromethane
10. customdried at 50-60° C.