HRID1199897

反应详情

EQUATION

反应方程式

HRID 1199897 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

26.5 g (0.1 mol) of 1-bromo-3-methyl-3-trifluoromethylthio-butan-2-one were added dropwise to a mixture of 8.3 g (0.12 mol) of 1,2,4-triazole and 28 g (0.2 mol) of potassium carbonate in 150 ml of acetone at room temperature. The mixture was subsequently stirred under reflux for 1 hour, the inorganic salts were filtered off and the filtrate was concentrated. The residue was taken up in methylene chloride, washed with water, dried over sodium sulphate and distilled. 15.5 g (62% of theory) of 3-methyl-1-(1,2,4-triazol-1-yl)-3-trifluoromethylmercaptobutan-2-one of boiling point 91° C./0.5 mm Hg and of melting point ~45° C. were obtained.

WORKUP

后处理

  1. temperatureunder reflux for 1 hour
  2. filtrationthe inorganic salts were filtered off
  3. concentrationthe filtrate was concentrated
  4. washwashed with water
  5. dry with materialdried over sodium sulphate
  6. distillationdistilled