HRID1577485

反应详情

EQUATION

反应方程式

HRID 1577485 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A sample of 3-[(1-ethylpropyl)amino]-6-methyl-2,4-dinitrobenzyl acetate (23.1 g; 0.068 mol) is added to a mixture of concentrated hydrochloric acid (30 ml), water (40 ml) and methanol (320 ml). The reaction mixture is refluxed for 4 hours, cooled down and concentrated in vacuo. It is then diluted with water, extracted with ether, and the ether layer dried. The ether is removed in vacuo to leave a red oil, which readily solidifies to a yellow-orange solid (19.9 g; 98.5%). A similarly prepared and purified sample has a melting point of 51°-54° C.

WORKUP

后处理

  1. temperatureThe reaction mixture is refluxed for 4 hours
  2. temperaturecooled down
  3. concentrationconcentrated in vacuo
  4. additionIt is then diluted with water
  5. extractionextracted with ether
  6. dry with materialthe ether layer dried
  7. customThe ether is removed in vacuo
  8. customto leave a red oil, which
  9. customA similarly prepared
  10. custompurified sample