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
The compound (837 mg, 2.53 mmol) obtained in step B was added to ethanol (20 ml), hydrazine monohydrate (0.31 ml, 6.4 mmol) was added, and the mixture was heated under reflux for 1 hr. The reaction mixture was cooled, and diethyl ether was added to allow precipitation of a solid. The precipitated solid was filtered, and the obtained solution was concentrated under reduced pressure to give a colorless oil. The oil was dissolved in diethyl ether, 4N hydrochloric acid-dioxane solution (1 ml) was added at room temperature and the mixture was diluted with ethyl acetate to allow precipitation of a solid. This was filtered, washed with ethyl acetate, and dried under reduced pressure to give the title compound (598 mg, yield 100%) as a colorless solid.
WORKUP
后处理
- additionwas added
- temperaturethe mixture was heated
- temperatureunder reflux for 1 hr
- temperatureThe reaction mixture was cooled
- customprecipitation of a solid
- filtrationThe precipitated solid was filtered
- concentrationthe obtained solution was concentrated under reduced pressure
- customto give a colorless oil
- customprecipitation of a solid
- filtrationThis was filtered
- washwashed with ethyl acetate
- customdried under reduced pressure