HRID1401416
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
Sulfuric acid is added to a solution of 4-fluorophenyl hydrazine hydrochloride (1 equiv.) in dioxane and stirred for 5 min. at RT. N-Methyl piperidone (0.76-1.4 equiv.) is added and the mixture is heated at 80° C. for 2 h. After completion, as monitored by TLC, the reaction mixture is concentrated under reduced pressure and basified to pH 10 using 10% aqueous KOH solution. The reaction mixture is extracted with EtOAc, dried over anhydrous sodium sulfate and concentrated under reduced pressure using rotary evaporator to provide the desired compound.
WORKUP
后处理
- temperaturethe mixture is heated at 80° C. for 2 h
- concentrationthe reaction mixture is concentrated under reduced pressure and basified to pH 10
- extractionThe reaction mixture is extracted with EtOAc
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
- customevaporator