HRID723552

反应详情

EQUATION

反应方程式

HRID 723552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Aluminum chloride (26.0 g, 195 mmol) was added in portions to a solution of 4-nitrobenzoyl chloride (27.8 g, 150 mL) and 4-fluorobenzene (15.8 g, 165 mmol) in carbon disulfide (100 mL). After 1 hour, the resulting yellow mixture was carefully treated with concentrated hydrochloric acid (60 mL) and stirred for 30 minutes. The mixture was then diluted with water and extracted with ethyl acetate. The organic layer was washed with dilute sodium hydroxide solution, water and brine, dried (MgSO4), and the solvent removed in vacuo. Crystallization from ethyl ether/hexanes gave 4-(4-fluorobenzoyl)-nitrobenzene (10.6 g, 82%) as a white solid, m.p. 87–88° C.; Analysis for C13H8NO3F: Calc.: C, 63.69; H, 3.26; N, 5.7: Found: C, 63.89; H, 3.28; N, 5.78.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with dilute sodium hydroxide solution, water and brine
  3. dry with materialdried (MgSO4)
  4. customthe solvent removed in vacuo
  5. customCrystallization from ethyl ether/hexanes