反应详情

A solution of 4.7 g of 4-(1H-indazol-3-yl)piperidine-1-carboximidic acid methyl ester and 80% of acetic acid was heated under reflux for 48 hrs. The reaction mixture was cooled and poured into water. The aqueous phase was extracted with ether and then made basic by the slow addition of a 50% aqueous sodium hydroxide solution. A solid separated from the solution. The solid was collected and dried. Recrystallization from ethanol yielded 1.7 g (46%) of product. Concentration of the mother liquors from this and another experiment gave additional product, mp 213°-215° C.

1. temperatureunder reflux for 48 hrs
2. temperatureThe reaction mixture was cooled
3. extractionThe aqueous phase was extracted with ether
4. additionmade basic by the slow addition of a 50% aqueous sodium hydroxide solution
5. customA solid separated from the solution
6. customThe solid was collected
7. customdried
8. customRecrystallization from ethanol