反应详情

To a solution of N-Boc-4-(4-ethyl-piperazin-1-yl)-2,6-difluoro-phenylamine (2.4 g, 7.03 mmol) obtained in Step B in ethyl acetate (20 ml), 6M−HCl aqueous solution (10 ml) was added, followed by stirring at room temperature for 1 hour. To this, 5M-NaOH aqueous solution was added to adjust the pH to 8, followed by extraction with ethyl acetate (50 ml×2). The organic layer was dried over sodium sulfate, and the solvent was distilled off under reduced pressure. This was purified by silica gel column chromatography (dichloromethane/methanol=50/1 to 20/1), followed by further dissolution in a minimum amount of dichloromethane. n-Hexane was added, and an oily component was removed, to obtain the desired compound as a brown solid (1.33 g, 78%).

1. extractionfollowed by extraction with ethyl acetate (50 ml×2)
2. dry with materialThe organic layer was dried over sodium sulfate
3. distillationthe solvent was distilled off under reduced pressure
4. customThis was purified by silica gel column chromatography (dichloromethane/methanol=50/1 to 20/1)
5. dissolutionfollowed by further dissolution in a minimum amount of dichloromethane
6. additionn-Hexane was added
7. customan oily component was removed