反应详情

To a suspension of 4-{2-[2-(acetylamino)-1,3-thiazol-4-yl]ethyl}-2-fluorobenzyl tert-butyl hydrazine-1,2-dicarboxylate (147.0 mg, 0.325 mmol) in anhydrous dichloromethane (2 ml) was added 4M hydrogen chloride dioxane solution (2 ml). After stirring at room temperature for 2 hr, and the mixture was concentrated under reduced pressure. Ethyl acetate was added to the concentrated residue, and the mixture was concentrated again under reduced pressure. This operation was performed 3 times to remove hydrogen chloride gas azeotropically. The residue was suspended in a mixture of ethanol (2 ml) and ethyl acetate (8 ml) and filtered. The filtered product was washed twice with ethyl acetate, and dried under reduced pressure to give 4-{2-[2-(acetylamino)-1,3-thiazol-4-yl]ethyl}-2-fluorobenzyl hydrazinecarboxylate hydrochloride (129.1 mg, quantitative) as a white solid.

1. concentrationthe mixture was concentrated under reduced pressure
2. additionEthyl acetate was added to the concentrated residue
3. concentrationthe mixture was concentrated again under reduced pressure
4. customto remove hydrogen chloride gas azeotropically
5. additionThe residue was suspended in a mixture of ethanol (2 ml) and ethyl acetate (8 ml)
6. filtrationfiltered
7. washThe filtered product was washed twice with ethyl acetate
8. customdried under reduced pressure