HRID472016

反应详情

EQUATION

反应方程式

HRID 472016 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 3-hydroxytetrahydrofuran (2.57 ml, 1.2 eq, 23.0 mmol) in THF (50 ml) was added sodium hydride as a 60% dispersion in oil (0.84 g, 1.1 eq, 20.91 mmol) this mixture was then stirred at 0° C. for 30 minutes. The preceding mixture was added dropwise to a solution of 3-fluoro-4-nitrobenzamide (3.5 g, 1.0 eq, 19.01 mmol) in THF (30 ml) and stirred at room temperature for 3.5 hours. The reaction was quenched with water and extracted with DCM (3×50 ml), the organics were combined, dried over sodium sulphate, filtered and the solvent removed in vacuo to give the title compound as a yellow solid (4.77 g, 18.9 mmol, 96% corrected). LCMS: [M+H]+=253, Rt=1.41 min, 100% purity

WORKUP

后处理

  1. stirringstirred at room temperature for 3.5 hours
  2. customThe reaction was quenched with water
  3. extractionextracted with DCM (3×50 ml)
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. customthe solvent removed in vacuo