反应详情

To N-(1-benzoyl-4-piperidinyl)-2-(2-carbamoylethyl)aniline (85 g) prepared in Reference Example 4 is added 5 % hydrochloric acid (500 ml) and the mixture is refluxed for 5 hours. After cooling, the reaction mixture is extracted with diethyl ether and the aqueous layer is made alkaline with a 50 % aqueous sodium hydroxide solution and extracted with ethyl acetate. The extract is dried over sodium carbonate and concentrated. The concentrate is purified by silica gel column chromatography (eluent; n-hexane/ethyl acetate=1/0-10/1) and recrystallized from ethanol/n-hexane to give 1-(1-benzoyl-4-piperidinyl)-3,4-dihydrocarbostyril (35 g) as white powders, m.p. 108°-111° C.

1. temperaturethe mixture is refluxed for 5 hours
2. temperatureAfter cooling
3. extractionthe reaction mixture is extracted with diethyl ether
4. extractionextracted with ethyl acetate
5. dry with materialThe extract is dried over sodium carbonate
6. concentrationconcentrated
7. customThe concentrate is purified by silica gel column chromatography (eluent; n-hexane/ethyl acetate=1/0-10/1)
8. customrecrystallized from ethanol/n-hexane