HRID883040

反应详情

EQUATION

反应方程式

HRID 883040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To N-(3-isopropyl-phenyl)-4-methyl-3-nitro-benzamide (3.0 g, 0.010 mol) dissolved in EtOAc (60 mL) in a 100 mL RBF was added Pd/C (10%, 250 mg). The flask was capped with a rubber septum and flushed with H2 gas through a balloon/needle. Positive H2 pressure was applied through the balloon/needle and reaction was stirred vigorously at room temperature for 3 days. TLC indicated clean conversion of starting material. The reaction was filtered through a pad of sand/celite. After concentration, the mixture was purified by silica gel chromatography to afford a light orange oil. Trituration with a mixture of hexanes and EtOAc afforded 3-amino-N-(3-isopropyl-phenyl)-4-methyl-benzamide as an off-white solid. MS m/z 269=[M+H]+. Calc'd for C17H20N2O: 268.36.

WORKUP

后处理

  1. customThe flask was capped with a rubber septum
  2. customflushed with H2 gas through a balloon/needle
  3. customPositive H2 pressure was applied through the balloon/needle and reaction
  4. filtrationThe reaction was filtered through a pad of sand/celite
  5. concentrationAfter concentration
  6. customthe mixture was purified by silica gel chromatography
  7. customto afford a light orange oil