反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a suspension of 4-{2-[2-(acetylamino)-1,3-thiazol-4-yl]ethyl}benzyl tert-butyl hydrazine-1,2-dicarboxylate (203.0 mg, 0.467 mmol) in anhydrous dichloromethane (2.3 ml) was added 4M hydrogen chloride dioxane solution (2.3 ml, 9.2 mmol). After stirring at room temperature for 2.5 hr, 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 ethyl acetate and filtered. The filtered product was washed with ethyl acetate and dried under reduced pressure to give the title compound (179.3 mg, quantitative) as a white solid.
WORKUP
后处理
- concentrationthe mixture was concentrated under reduced pressure
- additionEthyl acetate was added to the concentrated residue
- concentrationthe mixture was concentrated again under reduced pressure
- customto remove hydrogen chloride gas azeotropically
- filtrationfiltered
- washThe filtered product was washed with ethyl acetate
- customdried under reduced pressure