反应详情

Combine 1-benzyl-(4-(pyridin-3-yl)-piperidine-4-carboxylic acid (2.5 g, 8.4 mmol) and morpholine (1.5 g, 16.9 mmol) in dimethylformamide (65 mL). Add 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDC) (2.2 g), 1-hydroxy-benzotriazole hydrate (HOBt) (1.6 g), and dimethylformamide (25 mL). After 24 hours, pour the reaction mixture into a saturated aqueous sodium bicarbonate solution and extract twice with diethyl ether. Combine the organic layers, dry over MgSO4, filter, and concentrate to about 50 mL to give solid. Collect the solid by filtration, rinse with diethyl ether, and dry to give 1-benzyl-(4-(pyridin-3-yl)-piperidine-4-carboxylic acid morpholine-amide: Rf =0.67 (silica gel, dichloromethane/methanol/concentrated ammonia 90/10/0.5).

1. extractionextract twice with diethyl ether
2. dry with materialdry over MgSO4
3. filtrationfilter
4. concentrationconcentrate to about 50 mL
5. customto give solid
6. customCollect the solid
7. filtrationby filtration
8. washrinse with diethyl ether
9. customdry