HRID386003

反应详情

EQUATION

反应方程式

HRID 386003 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

6-Chloronicotinaldehyde (500 mg, 3.53 mmol) was added to tetrahydrofuran (23 mL) and cooled to 0° C. Trimethyl(trifluoromethyl)silane (0.66 mL, 4.24 mmol) was added followed by 1 M tetra-n-butylammonium fluoride in tetrahydrofuran (4.24 mL, 4.24 mmol). The reaction mixture was allowed to warm to room temperature over 1 hour. The reaction was then diluted with water and brine and extracted with ethyl acetate three times. The organic layers were combined and dried over magnesium sulfate, filtered, and concentrated in vacuo. The concentrated material was purified via silica gel chromatography (0-40% ethyl acetate in hexanes) to afford the title compound.

WORKUP

后处理

  1. temperatureto warm to room temperature over 1 hour
  2. extractionextracted with ethyl acetate three times
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe concentrated material was purified via silica gel chromatography (0-40% ethyl acetate in hexanes)