反应详情

A mixture of 5.0 g of 4-(1,2-benzisoxazole-3-yl)-1-piperidine carboxylic acid phenyl ester, 100 ml of ethanol, 50 g of (85%) potassium hydroxide and 50 ml of water was heated under reflux, with stirring, under nitrogen for 16 hrs. Most of the ethanol was removed in vacuo and the resultant aqueous suspension was extracted with ether (3×50 ml). The ether extracts were combined, washed with water, dried over anhydrous magnesium sulfate and the ether removed under reduced pressure to give an oil. The oil was dissolved in anhydrous ether and hydrogen chloride was introduced to precipitate a 3.0 g of a hydrochloride salt. Recrystallization from methanol-ether gave 2.0 g (57%) of product as the hydrochloride, mp, 313°-315° (dec.).

1. temperaturewas heated
2. temperatureunder reflux
3. customMost of the ethanol was removed in vacuo
4. extractionthe resultant aqueous suspension was extracted with ether (3×50 ml)
5. washwashed with water
6. dry with materialdried over anhydrous magnesium sulfate
7. customthe ether removed under reduced pressure
8. customto give an oil
9. customto precipitate a 3.0 g of a hydrochloride salt
10. customRecrystallization from methanol-ether