反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
Glacial acetic acid (4.5 ml, 75 mmol) was added to a suspension of 6-amino-1-methyluracil (5.66 g, 50 mmol) in hot water (100 ml). Sodium nitrite (4.14 g) was added in portions and the reaction mixture was stirred for 1 hour. The precipitate was collected by filtration, washed with water (75 ml) and then suspended in water (100 ml). The mixture was warmed to 50° C. and sodium dithionite (10 g) was added in portions keeping the temperature of the reaction between 50-55° C. The mixture was stirred at 50° C. for 1 hr and then cooled to room temperature and filtered. The solid was washed with water (2×25 ml), acetone (2×25 ml) and dried under vacuum to provide 5,6-diamino-1-methyluracil (5.6 g).
WORKUP
后处理
- filtrationThe precipitate was collected by filtration
- washwashed with water (75 ml)
- additionsodium dithionite (10 g) was added in portions
- customthe temperature of the reaction between 50-55° C
- stirringThe mixture was stirred at 50° C. for 1 hr
- temperaturecooled to room temperature
- filtrationfiltered
- washThe solid was washed with water (2×25 ml), acetone (2×25 ml)
- customdried under vacuum