HRID449533

反应详情

EQUATION

反应方程式

HRID 449533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The procedure as disclosed in the literature (Simonis, H. Ber. Deut. Chem. Ges. 1901, 34, 509; U.S. Pat. No. 6,747,159) is used. 3.54 g of aniline are dissolved in 15 ml of ethanol in a 100 ml beaker. Separately, 5 g of mucobromic acid are dissolved in 15 ml of ethanol in a 100 ml Erlenmeyer flask. This solution is added dropwise to the aniline/ethanol solution, with cooling. The reaction mixture turns immediately yellow, then orange, with development of CO2. At the end of the addition, the mixture is heated in a water bath until its volume is reduced by one half. The resulting solution is cooled with an ice-salt mixture, forming a yellow crystalline precipitate. This solid is collected on a fritted glass filter to afford pure product 5; additional product 5 can be recovered from concentration and recrystallization of the mother liquor.

WORKUP

后处理

  1. temperaturewith cooling
  2. additionAt the end of the addition
  3. temperaturethe mixture is heated in a water bath until its volume
  4. customforming a yellow crystalline precipitate
  5. customThis solid is collected on a fritted glass
  6. filtrationfilter