反应详情

To a suspension of tert-butyl 2-[(4-{2-[5-(4-acetylpiperazin-1-yl)pyridin-2-yl]ethyl}benzyl)carbamoyl]hydrazinecarboxylate (121.0 mg, 0.243 mmol) in anhydrous dioxane (1.2 ml) was added 4M hydrogen chloride dioxane solution (1.2 ml). After stirring at room temperature for 5 hrs, the reaction mixture was concentrated under reduced pressure. Ethyl acetate (10 ml) was added to the residue, and the mixture was concentrated again under reduced pressure. This operation was performed 3 times to azeotropically remove hydrogen chloride gas. The residue was suspended in a mixture of ethanol (3 ml) and ethyl acetate (6 ml), filtered, washed with ethyl acetate and dried under reduced pressure to give the title compound (111.0 mg, yield 90.1%) as a slightly yellow solid.

1. concentrationthe reaction mixture was concentrated under reduced pressure
2. additionEthyl acetate (10 ml) was added to the residue
3. concentrationthe mixture was concentrated again under reduced pressure
4. additionThe residue was suspended in a mixture of ethanol (3 ml) and ethyl acetate (6 ml)
5. filtrationfiltered
6. washwashed with ethyl acetate
7. customdried under reduced pressure