HRID1279236

反应详情

EQUATION

反应方程式

HRID 1279236 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of thiazolo[4,5-b]pyridine-2-thiol (6.2 g, 0.037 mol) in N,N-dimethylformamide under nitrogen is treated with 1,1,2-trifluoro-4-bromobutene (8.3 g, 0.046 mol) and potassium carbonate (1.5 g), heated to and stirred at 60° C. for 24 hours, cooled, and poured into water. The resultant aqueous mixture is extracted with diethyl ether. The organic extract is dried over anhydrous sodium sulfate and concentrated in vacuo to obtain a residue. Column chromatography of the residue using silica gel and a 9:1 hexanes/ethyl acetate solution gives the title product as a colorless oil (8.9 g, 64% yield).

WORKUP

后处理

  1. temperatureheated to and
  2. temperaturecooled
  3. extractionThe resultant aqueous mixture is extracted with diethyl ether
  4. extractionThe organic extract
  5. dry with materialis dried over anhydrous sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customto obtain a residue