HRID1060337

反应详情

EQUATION

反应方程式

HRID 1060337 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

1-Iodo-3,5-dinitrobenzene (1.8 g, 6.1 mmol) are dissolved in methanol (12 ml) and treated with a solution of sodium methoxide in methanol (5.4M, 1.2 ml). The mixture is then stirred at 65° C. for 52 h. After cooling to ambient temperature, water (50 ml) is added and the mixture extracted three times with ethyl acetate (50 ml). The combined organic layers are extracted with brine (100 ml), dried and evaporated to dryness. Flash chromatography (silica, eluent ethyl acetate/cyclohexane 1:1) affords the product (1.7 g, 99%) as light yellow solid. MS: m/e=279 (M+).

WORKUP

后处理

  1. temperatureAfter cooling to ambient temperature
  2. extractionthe mixture extracted three times with ethyl acetate (50 ml)
  3. extractionThe combined organic layers are extracted with brine (100 ml)
  4. customdried
  5. customevaporated to dryness