HRID1839435

反应详情

EQUATION

反应方程式

HRID 1839435 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N-(3-cyanobenzoyl)-2-nitro-4-(dimethyl-t-butylsiloxy)aniline (5.00 g, 12.6 mmol), 10% Pd/C (2.5 g), EtOH (160 mL), and THF (160 mL) was hydrogenated at 1 atm for 12 h. The reaction was filtered through diatomaceous earth with hot methanolic washes. The filtrate was concentrated and chromatographed (20% EtOAc/hexanes to 30% EtOAc/hexanes) to give the title compound as a solid (2.72 g, 59%).

WORKUP

后处理

  1. filtrationThe reaction was filtered through diatomaceous earth with hot methanolic washes
  2. concentrationThe filtrate was concentrated
  3. customchromatographed (20% EtOAc/hexanes to 30% EtOAc/hexanes)