反应详情

A mixture of 5.2 g of 1-methyl-4-(2-fluorobenzoyl)piperidine, 2.5 g of hydroxylamine hydrochloride, 5.4 g of ammonium acetate and 50+15 ml of ethanol-water was heated under reflux for 22 hrs. Most of the ethanol was removed under reduced pressure. The aqueous mixture was made basic with aqueous sodium hydroxide and the mixture was extracted with chloroform. The chloroform extract was dried over anhydrous magnesium sulfate and the chloroform was evaporated in vacuo to give a solid. The solid was triturated with ether. Recrystallization from ethanol-water gave 3.0 g (52.6%) of product, mp, 136°-139°.

1. temperaturewas heated
2. temperatureunder reflux for 22 hrs
3. customMost of the ethanol was removed under reduced pressure
4. extractionthe mixture was extracted with chloroform
5. extractionThe chloroform extract
6. dry with materialwas dried over anhydrous magnesium sulfate
7. customthe chloroform was evaporated in vacuo
8. customto give a solid
9. customThe solid was triturated with ether
10. customRecrystallization from ethanol-water