HRID2057979
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
8.62 gm of 11-chloroacetyl-5,11-dihydro-6H-pyrido[2,3-b][1,4]-benzodiazepin-6-one, 3.5 gm of sodium carbonate and 5.07 gm of 1-(3-methyl-but-2-enyl)-piperazine [R1 =--CH2 --CH=C(CH3)2 ] were refluxed in 100 ml of isopropanol for 2.5 hours. Then, the reaction mixture was suction-filtered while still hot, and the filtrate evaporated to a volume of 40 ml and cooled. The precipitated crystals were dissolved, while heating, in 100 ml of absolute ethanol, and the calculated quantity of concentrated hydrochloric acid was added. Upon cooling, the dihydrochloride crystallized out.
WORKUP
后处理
- filtrationThen, the reaction mixture was suction-filtered while still hot, and the filtrate
- customevaporated to a volume of 40 ml
- temperaturecooled
- dissolutionThe precipitated crystals were dissolved
- temperaturewhile heating, in 100 ml of absolute ethanol
- additionthe calculated quantity of concentrated hydrochloric acid was added
- temperatureUpon cooling
- customthe dihydrochloride crystallized out