HRID365378

反应详情

EQUATION

反应方程式

HRID 365378 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

Phenol (1.89 g, 20 mmol) was added to a slurry of hexane-washed NaH (60% oil suspension, 820 mg, 20.5 mmol) in DMSO (20 mL), stirred under nitrogen at 20° C., producing strong gas evolution. After 30 minutes, 1-fluoro-4-nitrobenzene (2.82 g, 20 mmol) was added dropwise to the light grey slurry. After about 10 minutes, the reaction mixture became orange and quite strongly exothermic, and a lot of gas was evolved. After 2 hours, the reaction mixture was poured onto ice-water (200 mL), and the solid was collected by Buchner filtration, rinsed with water (2×50 mL), and air dried to give 4-nitrodiphenyl ether (3.945 g, 91.6%) as dull yellow crystals.

WORKUP

后处理

  1. customproducing strong gas evolution
  2. waitAfter about 10 minutes
  3. waitAfter 2 hours
  4. additionthe reaction mixture was poured onto ice-water (200 mL)
  5. filtrationthe solid was collected by Buchner filtration
  6. washrinsed with water (2×50 mL), and air
  7. customdried