HRID267677

反应详情

EQUATION

反应方程式

HRID 267677 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

p-Fluoronitrobenzene (14.1 grams; 0.1 mol) is dissolved in tetrahydrofuran (100 ml). Ten percent palladium on charcoal catalyst (0.1 gram) is added to the solution followed by hydrazine (6.0 ml; 0.1 mol), and the resulting mixture stirred at room temperature for about 48 hours with cooling as necessary. The reaction mixture, containing N-(4-fluorophenyl)hydroxylamine, is dried over anhydrous magnesium sulfate and filtered. To this solution is added trifluoromethyl isocyanate (11.1 grams; 0.1 mol) and the solution is stirred for about 15 minutes. The reaction mixture is concentrated by evaporation of solvent and the resulting precipitate is recovered by filtration to yield 1-trifluoromethyl-3-(4'-fluorophenyl)-3-hydroxyurea.

WORKUP

后处理

  1. temperaturewith cooling as necessary
  2. dry with materialis dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. stirringthe solution is stirred for about 15 minutes
  5. concentrationThe reaction mixture is concentrated by evaporation of solvent
  6. filtrationthe resulting precipitate is recovered by filtration