HRID1198117
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
2,4-Dichlorothieno[2,3-d]pyrimidine (2 g, 0.00975 mol) and N-methylaniline (5 ml) were heated in an oil bath at 150° for 2 hours. The reaction mixture was dissolved in chloroform (200 ml) and extracted with 2N hydrochloric acid (3×100 ml). The chloroform solution was then washed with sodium carbonate solution, dried over magnesium sulphate, filtered and evaporated to give an oil. The oil was purified by chromatography using dichloromethane as eluant. The solid obtained was recrystallized from ether/petroleum ether (b.p. 40°-60°) to give the title compound, (1.2 g) m.p. 85°-87°.
WORKUP
后处理
- extractionextracted with 2N hydrochloric acid (3×100 ml)
- washThe chloroform solution was then washed with sodium carbonate solution
- dry with materialdried over magnesium sulphate
- filtrationfiltered
- customevaporated
- customto give an oil
- customThe oil was purified by chromatography
- customThe solid obtained
- customwas recrystallized from ether/petroleum ether (b.p. 40°-60°)