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
CONDITIONS
反应条件
- 温度
- 10 °C
PROCEDURE
实验过程
(+)8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-on (100 g) was suspended in the mixture of ethanol (300 ml) and deionized water (300 ml), and 6 N hydrochloric acid (100 ml) was added thereto at an interior temperature of not less than 30° C. After the addition thereof, it was heated to an interior temperature of 65~75° C. and the precipitated crystals were dissolved. After the dissolution, it was clarified by filtration, and the filtration vessel and so forth were washed with 200 ml of deionized water. The filtrate and the washings was combined, cooled to a temperature of not higher than 10° C., and the precipitated crystals were collected by filtration, washed with water, and dried to obtain (+)8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-one·hydrochloride as white crystals.
WORKUP
后处理
- additionwas added
- customat an interior temperature of not less than 30° C
- additionAfter the addition
- temperatureit was heated to an interior temperature of 65~75° C.
- dissolutionthe precipitated crystals were dissolved
- dissolutionAfter the dissolution, it
- filtrationwas clarified by filtration
- washthe filtration vessel and so forth were washed with 200 ml of deionized water
- filtrationthe precipitated crystals were collected by filtration
- washwashed with water
- customdried