HRID1582176

反应详情

EQUATION

反应方程式

HRID 1582176 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Mercaptothiazole (5.18 g), potassium carbonate (6.72 g) and 4-bromo-1,1,2-trifluorobutene-1 (9.21 g) are refluxed in acetonitrile (60 ml) in the presence of argon gas for 6 hours by heating. After the reaction mixture has reached room temperature, it is filtered and the solvent is distilled off. The residue is dissolved in dichloromethane and washed with 5% aqueous solution of sodium hydroxide and water in this order. It is dried over unhydrous sodium sulfate and purified by column chromatography (eluent: dichloromethane) to obtain 2-(3,4,4-trifluoro-3-butenyl-thio)thiazole (8.6 g) as pale yellow liquid (n20D 1.5200).

WORKUP

后处理

  1. temperatureby heating
  2. customhas reached room temperature
  3. filtrationit is filtered
  4. distillationthe solvent is distilled off
  5. dissolutionThe residue is dissolved in dichloromethane
  6. washwashed with 5% aqueous solution of sodium hydroxide and water in this order
  7. dry with materialIt is dried over unhydrous sodium sulfate
  8. custompurified by column chromatography (eluent: dichloromethane)