HRID1470077
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
Into a 50-mL round-bottom flask, was placed a solution of diethyl 4-nitrophenylphosphonate (1.07 g, 4.13 mmol, 1.00 equiv), TEA (3 mL), Palladium carbon (0.025 g). This was followed by the addition of formic acid (2 mL) dropwise with stirring at room temperature. The resulting solution was heated to reflux for 3 hr. The reaction was then quenched by the addition of 5 mL, of water and the solids were filtered out. The resulting filtrate was extracted with 5×10 mL, of dichloromethane and the organic layers combined and dried over anhydrous sodium sulfate. This resulted in 800 mg (85%) of diethyl 4-aminophenylphosphonate as a white solid.
WORKUP
后处理
- customInto a 50-mL round-bottom flask, was placed
- temperatureThe resulting solution was heated
- temperatureto reflux for 3 hr
- customThe reaction was then quenched by the addition of 5 mL, of water
- filtrationthe solids were filtered out
- extractionThe resulting filtrate was extracted with 5×10 mL, of dichloromethane
- dry with materialdried over anhydrous sodium sulfate
- customThis resulted in 800 mg (85%) of diethyl 4-aminophenylphosphonate as a white solid