Hydrochloric Acid → N-[2,4-difluoro-5-(4-piperidinyl)phenyl]-2-methylpropanamide
반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([NH:9][C:10](=[O:14])[CH:11]([CH3:13])[CH3:12])=[CH:4][C:3]=1[CH:15]1[CH2:20][CH2:19][N:18](C(OC(C)(C)C)=O)[CH2:17][CH2:16]1.Cl>O1CCOCC1>[F:8][C:6]1[CH:7]=[C:2]([F:1])[C:3]([CH:15]2[CH2:16][CH2:17][NH:18][CH2:19][CH2:20]2)=[CH:4][C:5]=1[NH:9][C:10](=[O:14])[CH:11]([CH3:12])[CH3:13]참가 물질
4
실험 절차
Into a solution of tert-butyl 4-[2,4-difluoro-5-(isobutyrylamino)phenyl]-1-piperidinecarboxylate (6.54 g, 17.1 mmol) in 1,4-dioxane (40.0 mL) was added 4M HCl in 1,4-dioxane (160 mL) at room temperature. The reaction mixture was stirred for 1 h and concentrated in vacuo. The residue was dissolved in 100 mL of H2O and was basified with 10% KOH solution (50 mL). The aqueous layer was extracted with CHCl3/i-PrOH (3:1, 3×150 mL). The combined organic extracts were washed with brine, dried over MgSO4, filtered and concentrated in vacuo to give 4.72 g (16.7 mmol, 98%) of N-[2,4-difluoro-5-(4-piperidinyl)phenyl]-2-methylpropanamide: ESMS m/e: 283.3 (M+H)+.