HRID61606

反应详情

EQUATION

反应方程式

HRID 61606 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 4,5-dimethoxy-2-nitrobenzamide (5.8 g, 25.6 mmol) in a 1:1 mixture of DME/MeOH (total volume 200 ml) and 10% Pd/C (0.7 g) was hydrogenated at RT using a balloon filled with hydrogen gas. The reaction was stirred for 16 h and the reaction mixture filtered through Celite®. The pad of Celite® was washed with a 1:1 mixture of MeOH/CH2Cl2 (200 mL). The filtrate was then concentrated in vacuo and dried under high vacuum overnight to give 2-amino-4,5-dimethoxybenzamide. (5.0 g, 25.5 mmol, 99%). HPLC retention time 2.303 mins.

WORKUP

后处理

  1. customwas hydrogenated at RT
  2. filtrationthe reaction mixture filtered through Celite®
  3. washThe pad of Celite® was washed with a 1:1 mixture of MeOH/CH2Cl2 (200 mL)
  4. concentrationThe filtrate was then concentrated in vacuo
  5. customdried under high vacuum overnight