HRID1814917

反应详情

EQUATION

反应方程式

HRID 1814917 的结构方程式

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 (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

  1. filtrationThe precipitate was collected by filtration
  2. washwashed with water (75 ml)
  3. additionsodium dithionite (10 g) was added in portions
  4. customthe temperature of the reaction between 50-55° C
  5. stirringThe mixture was stirred at 50° C. for 1 hr
  6. temperaturecooled to room temperature
  7. filtrationfiltered
  8. washThe solid was washed with water (2×25 ml), acetone (2×25 ml)
  9. customdried under vacuum