反应详情

Step AAH (5): To a soln of 3-oxo-N-phenyl-6-(2-phenyl-1,3-dioxolan-2-yl)hexanamide (444 mg, 1.256 mmol) in THF (1 mL) was added hydrazine (0.059 mL, 1.88 mmol). The mixture was stirred at rt for 2 h, then at 65° C. for 2 h. The reaction mixture was concentrated in vacuo. Dichloromethane (10 mL) was added to the crude residue. After cooling to 0° C., the product crystallized out. The solid was collected by vacuum filtration and dried under high vacuum to afford 3-(3-(2-phenyl-1,3-dioxolan-2-yl)propyl)-1H-pyrazol-5(4H)-one (250 mg, 73% yield). LC-MS (M+H)+ 275.1.

1. waitat 65° C. for 2 h
2. concentrationThe reaction mixture was concentrated in vacuo
3. additionDichloromethane (10 mL) was added to the crude residue
4. temperatureAfter cooling to 0° C.
5. customthe product crystallized out
6. filtrationThe solid was collected by vacuum filtration
7. customdried under high vacuum