反应详情

To a mixture of 1-[(pyridin-3 yloxy)carbonyl]piperidine-4-carboxylic acid (1.5 g) and DCM (15 mL) were added 1-hydroxybenzotriazole (HOBt) (0.85 g), benzohydrazine (0.86 g), and 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide (WSC) hydrochloride (1.21 g), followed by stirring at room temperature for about 15 hours. To the reaction liquid were added chloroform and water, and the organic phase was separated. The organic phase was washed with water and saturated brine, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (chloroform/methanol=100/0 to 90/10). To the purified product were added diisopropyl ether and methanol, and the resulting solid was collected by filtration and dried under reduced pressure to obtain pyridin-3-yl 4-[(2-benzoylhydrazino)carbonyl]piperidine-1-carboxylic acid (1.22 g).

1. customTo the reaction liquid
2. customthe organic phase was separated
3. washThe organic phase was washed with water and saturated brine
4. dry with materialdried over magnesium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customthe residue was purified by silica gel column chromatography (chloroform/methanol=100/0 to 90/10)
7. additionTo the purified product were added diisopropyl ether and methanol
8. filtrationthe resulting solid was collected by filtration
9. customdried under reduced pressure