HRID476917

反应详情

EQUATION

反应方程式

HRID 476917 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.92 g of sodium was dissolved in 50 ml of absolute ethanol, and 6.40 g (53 mmol) of guanidine nitrate was added thereto. The solution was stirred for 10 minutes and filtered with Celite filter aid. 0.98 g (4.6 mmol) of 6-amino-1,3-diethyl-5-formyluracil was added to the filtrate and the reaction mixture was refluxed for 24 hours. After removal of the solvent under reduced pressure, 30 ml of water was added thereto. The crystalline precipitate was filtered off and recrystallized from ethanol to give 0.94 g of 7-amino-1,3-diethyl-pyrimido[4,5-d]pyrimidine-2,4-dione (compound 17) in a 87% yield.

WORKUP

后处理

  1. filtrationfiltered with Celite
  2. filtrationfilter aid
  3. temperaturethe reaction mixture was refluxed for 24 hours
  4. customAfter removal of the solvent under reduced pressure, 30 ml of water
  5. additionwas added
  6. filtrationThe crystalline precipitate was filtered off
  7. customrecrystallized from ethanol