HRID1391534

反应详情

EQUATION

反应方程式

HRID 1391534 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N-Methoxy-2-methyl-5-nitrobenzenesulfonamide (0.5 g, 2 mmol) was combined with 10% palladium on carbon (0.05 g), ethanol (10 mL), and hydrazine (1 mL) and heated at reflux for 18 h. The solution was filtered through celite, concentrated, and purified on silica gel with methanol in dichloromethane. Product was an off white solid (0.28 g, 1.3 mmoL). 1H NMR (300 MHz, d6-DMSO) δ10.3 (s, 1H), 7.11 (s, 1H), 7.02 (d, J=8.2 Hz, 1H), 6.7 (d, J=8.2 Hz, 1H), 5.37 (s, 2H), 3.57 (s, 3H), 2.38 (s, 3H).

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 18 h
  3. filtrationThe solution was filtered through celite,
  4. concentrationconcentrated
  5. custompurified on silica gel with methanol in dichloromethane