反应详情

A solution of 0.52 g of paraformaldehyde, 3.0 g of 3-(1-methyl-4-piperidinyl)-1H-indazole, 15 ml of ethanol and 0.34 ml of 5% aqueous sodium hydroxide was refluxed for 3 hrs. The ethanol was removed in vacuo and the residue diluted with water. The aqueous suspension was extracted with dichloromethane (2×, 50 ml) and the combined extracts were washed with water and dried over anhydrous magnesium sulfate. The dichloromethane was evaporated in vacuo to yield an oil, which crystallized upon standing. The solid was recrystallized twice from ethyl acetate to yield 1.3 g (57.8%) of product, mp 128°-130° C.

1. customThe ethanol was removed in vacuo
2. additionthe residue diluted with water
3. extractionThe aqueous suspension was extracted with dichloromethane (2×, 50 ml)
4. washthe combined extracts were washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe dichloromethane was evaporated in vacuo
7. customto yield an oil, which
8. customcrystallized
9. customThe solid was recrystallized twice from ethyl acetate