HRID384107

反应详情

EQUATION

反应方程式

HRID 384107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of 2-phenoxynicotinic acid (2.0 g) in tetrahydrofuran (20 ml), 9.5 ml of borane-tetrahydrofuran complex (1.17M tetrahydrofuran solution) was added, and the reaction solution was stirred overnight at 50° C. The reaction solution was cooled, 14 ml of 1N aqueous sodium hydroxide was added under ice-cooling, and the reaction solution was stirred for 1 hour. The reaction solution was diluted with saturated aqueous ammonium solution, extracted with diethyl ether, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue obtained was purified by silica gel column chromatography (eluent: ethyl acetate/hexane (0:100-50:50)) to afford the title compound as a colorless oil.

WORKUP

后处理

  1. temperatureThe reaction solution was cooled
  2. temperaturecooling
  3. stirringthe reaction solution was stirred for 1 hour
  4. extractionextracted with diethyl ether
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off under reduced pressure
  7. customthe residue obtained
  8. customwas purified by silica gel column chromatography (eluent: ethyl acetate/hexane (0:100-50:50))