HRID921348

反应详情

EQUATION

反应方程式

HRID 921348 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a pressure vessel was added 1-(3-methoxy-4-nitrophenyl)-4-methyl-1,4-azaphosphinane 4-oxide (272 mg, 0.960 mmol), ethanol (5 mL), and 10% Pd/C (50 mg). The vessel was connected to a Parr apparatus, evacuated, and refilled with nitrogen. The vessel was then evacuated and filled with hydrogen gas to a pressure of 50 psi. The reaction mixture was shaken under 50 psi for 4 h. The mixture was filtered through Celite to a flask containing HCl in ethanol. Concentration of the filtrate afforded 2-methoxy-4-(4-methyl-4-oxido-1,4-azaphosphinan-1-yl)aniline as a gray solid (211 mg, 87% yield).

WORKUP

后处理

  1. customevacuated
  2. additionrefilled with nitrogen
  3. customThe vessel was then evacuated
  4. additionfilled with hydrogen gas to a pressure of 50 psi
  5. filtrationThe mixture was filtered through Celite to a flask
  6. additioncontaining HCl in ethanol