HRID1606458
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
A mixture of 0.20 g. of 55% sodium hydride-mineral oil dispersion and 0.3 g. of dimethylaminoethylchloride hydrochloride in 12 ml. of dry dimethylformamide is stirred at room temperature for 0.5 hours. To the mixture is added 0.23 g. of 5,10-dihydro-10-methyl-6H-pyrido[3,2-b]thieno[3,4-e] [1,4]diazepin-6-one and stirring is continued for 18 hours. The reaction mixture is cooled, quenched with water and extracted with chloro form. The dried chloroform extracts are concentrated to give an amber oil, which is crystallized from hexane to give an off-white solid, m.p. 129°-130°C.
WORKUP
后处理
- additionA mixture of 0.20 g
- additionTo the mixture is added 0.23 g
- temperatureThe reaction mixture is cooled
- customquenched with water
- extractionextracted with chloro form
- concentrationThe dried chloroform extracts are concentrated
- customto give an amber oil, which
- customis crystallized from hexane
- customto give an off-white solid, m.p. 129°-130°C.