HRID1378219
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
1.37 g (3.18 mmol) of 7-chloro-8-fluoro-5-methyl-3-(5-piperidin-1-ylmethyl-1,2,4-oxadiazol-3-yl)-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one were dissolved in 50 ml of hot ethanol and treated at 40° with 0.95 ml (3.5 mol) of 3.7N ethanolic hydrochloric acid. After stirring at 0° for 30 minutes the solution was concentrated to a volume of ~20 ml and treated with 100 ml of ether. The white suspension obtained was suction filtered. There were obtained 1.30 g (88%) of 7-chloro-8-fluoro-5-methyl-3-(5-piperidin-1-ylmethyl-1,2,4-oxadiazol-3-yl)-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one hydrochloride (1:1) as white crystals; m.p. 240°-243° (dec.).
WORKUP
后处理
- concentrationwas concentrated to a volume of ~20 ml
- additiontreated with 100 ml of ether
- customThe white suspension obtained
- filtrationfiltered