HRID1528676

反应详情

EQUATION

反应方程式

HRID 1528676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

156 mg (about 66% pure, 0.636 mmol) of the compound from example 6A were dissolved in DMF (3.5 ml), 28 mg (0.70 mmol) of sodium hydride (60% in mineral oil) were then added and the mixture was stirred at RT for 2 h. 115 mg (0.604 mmol) of 2-chloro-5-nitropyrimidine-4,6-diamine (synthesis: Helvetica Chimica Acta (1951), 34, 835-40) were then added, and the reaction mixture was stirred at 80° C. for another 1 h. After cooling to RT, the mixture was added to water. The suspension obtained in this manner was filtered off and the solid was washed repeatedly with water and then dried under high vacuum. This gave 196 mg (77% of theory) of the title compound in solid form.

WORKUP

后处理

  1. stirringthe reaction mixture was stirred at 80° C. for another 1 h
  2. temperatureAfter cooling to RT
  3. customThe suspension obtained in this manner
  4. filtrationwas filtered off
  5. washthe solid was washed repeatedly with water
  6. customdried under high vacuum