HRID1936665

反应详情

EQUATION

反应方程式

HRID 1936665 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A cool (0° C.) solution of 7-(3-methylthiopropylamino)-4-oxo-2-(2-propoxyphenyl)-3,4-dihydropyrimido[4,5-d]pyrimidine (1.84 g) and m-chloroperoxybenzoic acid (0.97 g) in dichloromethane (180 ml) was allowed to warm to ambient temperature with stirring. The solution was then stirred for 18 hours at ambient temperature and allowed to stand for 10 days. The reaction mixture was evaporated under reduced pressure and the residue eluted from a silica column with chloroform:methanol (gradient elution). The combined fractions containing product were evaporated under reduced pressure and the residue was recrystallized from isopropanol to yield the title compound, 1.73 g, m.p. 188-9° C.

WORKUP

后处理

  1. stirringThe solution was then stirred for 18 hours at ambient temperature
  2. customThe reaction mixture was evaporated under reduced pressure
  3. washthe residue eluted from a silica column with chloroform
  4. additionThe combined fractions containing product
  5. customwere evaporated under reduced pressure
  6. customthe residue was recrystallized from isopropanol