HRID1107316
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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 recrystallized twice from ethanol to yield the title compound, 0.31 g, m.p. 235-236° C.
WORKUP
后处理
- customThe reaction mixture was evaporated under reduced pressure
- customto yield a cream solid which
- washThe organic solution was washed with water
- dry with materialdried (magnesium sulphate)
- customevaporated under reduced pressure
- customto yield a cream solid
- washElution from silica with chloroform:methanol (25:1)
- customyielded a crude product which
- customwas recrystallized twice from ethanol