HRID2235526

反应详情

EQUATION

反应方程式

HRID 2235526 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A suspension of 2,6-dinitrophenol 5.0 g (27 mmol), ammonium hydroxide (3 ml) and ammonium chloride 14.3 g (270 mmol) in 30 ml of water was heated to 70° C. A solution of sodium sulfide nonahydrate (24.19 g, 100 mmol) in water was added and the resulting mixture stirred at 70° C. for 2 h. The reaction was cooled to room temperature, acidified (pH 3.2) with 2N HCl, and the brown precipitate separated by filtration. The filtrate was extracted with chloroform (6×75 ml), the organic extracts combined with the precipitate, and evaporated in-vacuo to yield 2.5 g (60%) of product as a dark brown solid.

WORKUP

后处理

  1. temperatureThe reaction was cooled to room temperature
  2. customthe brown precipitate separated by filtration
  3. extractionThe filtrate was extracted with chloroform (6×75 ml)
  4. customevaporated in-vacuo