反应详情

温度

80 °C

To N-[3-(4-ethyl-piperazin-1-yl)-phenyl]-N-methyl-acetamide (104.9 mg) obtained in Step C, water (2 ml) and concentrated sulfuric acid (0.4 ml) were added, followed by stirring at 80° C. for 8 hours. To this, 5M-NaOH aqueous solution was added, to adjust the pH to 9, followed by extraction with ethyl acetate (10 ml×2), and the organic layer was dried over sodium sulfate. The sodium sulfate was filtered off, followed by purification by silica gel column chromatography (dichloromethane/methanol=20/1 to 10/1), to obtain the desired compound (76.1 mg, 86%).

1. extractionfollowed by extraction with ethyl acetate (10 ml×2)
2. dry with materialthe organic layer was dried over sodium sulfate
3. filtrationThe sodium sulfate was filtered off
4. customfollowed by purification by silica gel column chromatography (dichloromethane/methanol=20/1 to 10/1)