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
Ethyl 4-{3-{4-(4-ethylphenyl)methylamino-3-{3-[4-(2-methoxyphenyl)piperazin-1-yl]propoxy}benzoyl}indol-1-yl}butanoate hydrochloride (40.8 g) was dissolved in tetrahydrofuran (200 ml), and methanol (200 ml) and potassium hydroxide (11.3 g) were added to the solution. The resultant mixture was refluxed for one hour and 30 minutes. The reaction mixture was cooled and concentrated under reduced pressure. Water (1.2 l) was added to dilute the residue, and the resultant solution was poured into 1N hydrochloric acid (400 ml), to thereby precipitate crystals. The crystals were collected by filtration. The collected crystals were washed with water, dried, and recrystallized from 95% ethanol, to thereby obtain 33.8 g of 4-{3-{4-(4-ethylphenyl)methylamino-3-{3-[4-(2-methoxyphenyl)piperazin-1-yl]propoxy}benzoyl}indol-1-yl}butanoate hydrochloride as pale yellow crystals.
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- concentrationconcentrated under reduced pressure
- additionWater (1.2 l) was added
- additionto dilute the residue
- additionthe resultant solution was poured into 1N hydrochloric acid (400 ml)
- customto thereby precipitate crystals
- filtrationThe crystals were collected by filtration
- washThe collected crystals were washed with water
- customdried
- customrecrystallized from 95% ethanol