HRID1075328

反应详情

EQUATION

反应方程式

HRID 1075328 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 2-methyl-5-nitrobenzyl ether (11.5 g) is dissolved in absolute ethanol (125 ml). A solution of sodium sulfide monohydrate (48.3 g) and sodium bicarbonate (16.7 g) in water (75 ml) is added to the alcoholic solution. The resulting mixture is refluxed until thin layer chromatography indicates that the starting material is exhausted. The reaction mixture is then concentrated under vacuum to an oily solid. Methylene chloride is added and the mixture filtered. The methylene chloride layer is separated, dried, and is concentrated under vacuum to yield 9.3 g of a mobile orange liquid.

WORKUP

后处理

  1. temperatureThe resulting mixture is refluxed until thin layer chromatography
  2. concentrationThe reaction mixture is then concentrated under vacuum to an oily solid
  3. additionMethylene chloride is added
  4. filtrationthe mixture filtered
  5. customThe methylene chloride layer is separated
  6. customdried
  7. concentrationis concentrated under vacuum