HRID2042744
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
Hydrazine hydrate (5 mL) was added to a solution of Example 93C (1.07 g, 2.96 mmol) in dioxane (10 mL). The resulting solution was refluxed for 3 hours before it was cooled and partitioned with tetrahydrofuran and brine. The aqueous phase was acidified with 6 N hydrochloric acid to pH 2 and extracted repeatedly with a tetrahydrofuran/ethyl acetate mixture. The combined organic phases were dried (magnesium sulfate), filtered, and concentrated. The crude product was recrystallized from ethyl acetate and hexane to provide a light brown solid.
WORKUP
后处理
- temperatureThe resulting solution was refluxed for 3 hours before it
- temperaturewas cooled
- custompartitioned with tetrahydrofuran and brine
- extractionextracted repeatedly with a tetrahydrofuran/ethyl acetate mixture
- dry with materialThe combined organic phases were dried (magnesium sulfate)
- filtrationfiltered
- concentrationconcentrated
- customThe crude product was recrystallized from ethyl acetate and hexane
- customto provide a light brown solid