HRID372981

反应详情

EQUATION

反应方程式

HRID 372981 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7-Methylthio-4-oxo-2-(2-propoxyphenyl)-3,4-dihydropyrimido[4,5-d]pyrimidine (1.40 g) was treated with a solution of methylamine in industrial methylated spirit (33%; 30 ml) in a pressure vessel for 9 hours at 90° C. The reaction mixture was evaporated under reduced pressure to yield a cream solid which was dissolved in chloroform. The organic solution was washed with water, dried (magnesium sulphate) and evaporated under reduced pressure to yield a cream solid. Elution from silica with chloroform:methanol (25:1) yielded a crude product which was recrystallised twice from ethanol to yield the title compound, 0.31 g, m.p. 235°-236° C.

WORKUP

后处理

  1. customThe reaction mixture was evaporated under reduced pressure
  2. customto yield a cream solid which
  3. washThe organic solution was washed with water
  4. dry with materialdried (magnesium sulphate)
  5. customevaporated under reduced pressure
  6. customto yield a cream solid
  7. washElution from silica with chloroform:methanol (25:1)
  8. customyielded a crude product which
  9. customwas recrystallised twice from ethanol