反应详情

To methyl 4-[(2-{1-[5-(4-tert-butylphenyl)-4-hydroxy-1-methyl-1H-pyrazol-3-yl]ethylidene}hydrazino)carbonyl]-2-nitrobenzoate (0.945 mmol, 466.2 mg), methanol (33 mL) was added, and 1 M aqueous sodium hydroxide (4.7 mmol, 4.7 mL) was added. After about 26 hours of stirring at room temperature and 3 hours of stirring at 40° C., 1 M hydrochloric acid (4.7 mmol, 4.7 mL) and water were added. The precipitated solid was recovered by filtration, washed with water and dried by means of a vacuum pump. The resulting yellow solid (359.5 mg) was dissolved in THF (50 mL) and stirred at room temperature for 2 days. The insolubles were filtered off, and the filtrate was concentrated and dried by means of a vacuum pump. After addition of chloroform, the precipitated solid was recovered by filtration and dried by means of a vacuum pump to give the desired product as a pale yellow solid (260.7 mg, yield 58%).

1. stirringof stirring at 40° C.
2. filtrationThe precipitated solid was recovered by filtration
3. washwashed with water
4. customdried by means of a vacuum pump
5. dissolutionThe resulting yellow solid (359.5 mg) was dissolved in THF (50 mL)
6. stirringstirred at room temperature for 2 days
7. filtrationThe insolubles were filtered off
8. concentrationthe filtrate was concentrated
9. customdried by means of a vacuum pump
10. additionAfter addition of chloroform
11. filtrationthe precipitated solid was recovered by filtration
12. customdried by means of a vacuum pump