HRID372998

反应详情

EQUATION

反应方程式

HRID 372998 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 7-methylsulphonyl-4-oxo-2-(2-propoxyphenyl)-3,4-dihydropyrimido[4,5-d]pyrimidine (1.0 g), β-alanine ethyl ester hydrochloride (1.10 g) and triethylamine (0.73 g) in dichloromethane (20 ml) was stirred at ambient temperature for 2.5 hours. The reaction mixture was extracted with dilute hydrochloric acid (20 ml) then water (10 ml), and the extracts back washed with dichloromethane (10 ml). The combined organic extracts were dried (magnesium sulphate) and evaporated under reduced pressure to yield a crude product which was recrystallised from ethanol: water to yield the title compound, 0.83 g, m.p. 142°-3° C.

WORKUP

后处理

  1. extractionThe reaction mixture was extracted with dilute hydrochloric acid (20 ml)
  2. washwater (10 ml), and the extracts back washed with dichloromethane (10 ml)
  3. dry with materialThe combined organic extracts were dried (magnesium sulphate)
  4. customevaporated under reduced pressure
  5. customto yield a crude product which
  6. customwas recrystallised from ethanol