HRID719250
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 solution of 4-Piperazin-1-ylmethyl-benzoic acid (4c) and chloromethyl-phosphonic acid diethyl ester (4d) in ethanol was added potassium carbonate. The resulting reaction mixture was refluxed, then cooled to room temperature, diluted with brine, acidified to pH˜4, and extracted with EtOAc until the aqueous layer showed little or no evidence of product by HPLC. The combined organics were dried over MgSO4 and concentrated on rotary evaporator. The desired product was purified by silica gel flash chromatography.
WORKUP
后处理
- customThe resulting reaction mixture
- temperaturewas refluxed
- extractionextracted with EtOAc until the aqueous layer
- dry with materialThe combined organics were dried over MgSO4
- concentrationconcentrated on rotary evaporator
- customThe desired product was purified by silica gel flash chromatography