HRID1771638

反应详情

EQUATION

反应方程式

HRID 1771638 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

To a solution of 2-fluoro-5-(3-fluorophenyl)-N-(3-hydroxy-2,6-dimethyl-phenyl)benzamide (400 mg, 1.13 mmol, 1.0 eq) in THF under N2 was added dropwise a solution of BH3 (5.65 mL, 1M in THF, 5.65 mmol, 5.0 eq). The reaction mixture was heated to 60° C. and stirred under N2 for 3 h. After cooling, the resulting mixture was quenched by addition of 1 M HCl and water and the aqueous layer extracted with EtOAc. The organic extract was dried (Na2SO4), filtered, evaporated in vacuo and purified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:4) to give the title product as yellow oil (340 mg, 89%).

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe resulting mixture was quenched by addition of 1 M HCl and water
  3. extractionthe aqueous layer extracted with EtOAc
  4. extractionThe organic extract
  5. dry with materialwas dried (Na2SO4)
  6. filtrationfiltered
  7. customevaporated in vacuo
  8. custompurified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:4)