反应详情

A mixture of 13.3 g of 1-acetyl-4-(2-fluorobenzoyl)-4-hydroxypiperidine and 20 ml of 6N hydrochloric acid was stirred at reflux under nitrogen for 4 hrs. The reaction mixture was allowed to cool and poured onto ca. 100 g of ice. Methylene chloride was added, and the separated aqueous layer was made strongly basic by means of 15% sodium hydroxide solution. The aqueous layer was extracted three times with 80 ml of methylene chloride. The extracts were dried over anhydrous potassium carbonate, filtered and evaporated provide anhydrous 9.5 g (85%) of product, mp 133°-135° C.

1. temperatureat reflux under nitrogen for 4 hrs
2. temperatureto cool
3. extractionThe aqueous layer was extracted three times with 80 ml of methylene chloride
4. dry with materialThe extracts were dried over anhydrous potassium carbonate
5. filtrationfiltered
6. customevaporated