反应详情

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)+.

1. concentrationconcentrated in vacuo
2. dissolutionThe residue was dissolved in 100 mL of H2O
3. extractionThe aqueous layer was extracted with CHCl3/i-PrOH (3:1, 3×150 mL)
4. washThe combined organic extracts were washed with brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo