反应详情

Part D: To a stirred suspension of 1-(4-chlorophenyl)-5-phenyl-4,5-dihydro-(1H)-pyrazole-3-carboxylic acid (1.50 gram, 5 mmol) in anhydrous acetonitrile (40 ml) is successively added N-diisopropylethylamine (DIPEA) (1.92 ml, 11 mmol), O-benzotriazol-1-yl-N,N, N′,N′-tetramethyluronium hexafluorophosphate (HBTU) (2.08 g, 5.5 mmol) and 1-aminopiperidine (0.59 ml, 5.5 mmol) and the resulting mixture is reacted at room temperature for 16 hours in a N2 atmosphere. The mixture is concentrated and added to a mixture of ethyl acetate and aqueous NaHCO3. The Ethyl acetate layer is collected, dried over MgSO4, filtered and concentrated in vacuo. The resulting residue is recrystallised from acetonitrile to give N-(piperidin-1-yl)-1-(4-chlorophenyl)-5-phenyl-4,5-dihydro-(1H)-pyrazole-3-carboxamide (compound 1), 1.34 gram, 70% yield). Melting point: 189-192° C.

1. concentrationThe mixture is concentrated
2. additionadded to a mixture of ethyl acetate and aqueous NaHCO3
3. customThe Ethyl acetate layer is collected
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe resulting residue is recrystallised from acetonitrile