HRID870131

反应详情

EQUATION

反应方程式

HRID 870131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customInto a 50-mL round-bottom flask, was placed
  2. temperatureThe resulting solution was heated
  3. temperatureto reflux for 3 hr
  4. customThe reaction was then quenched by the addition of 5 mL of water
  5. filtrationthe solids were filtered out
  6. extractionThe resulting filtrate was extracted with 5×10 mL of dichloromethane
  7. dry with materialdried over anhydrous sodium sulfate
  8. customThis resulted in 800 mg (85%) of diethyl 4-aminophenylphosphonate as a white solid