反应 #1574

ord-b4cbb9aa494e49f7b3f195512e6252b9

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONpoured onto ice
  2. 2
    过滤The resultant aqueous mixture is filtered
  3. 3
    其他to obtain a tan solid which
  4. 4
    洗涤is washed with water
  5. 5
    其他dried overnight
  6. 6
    其他recrystallized from a chloroform/hexanes (17:1) solution

实验过程

A mixture of 4'-chloro-2'-fluoroacetanilide (51 g, 0.272 mol) in concentrated sulfuric acid (100 mL) is cooled to 0° C., treated with nitric acid (90% real, 14 mL, 0.300 mol) over 45 minutes, stirred for 10 minutes, and poured onto ice. The resultant aqueous mixture is filtered to obtain a tan solid which is washed with water, dried overnight, and recrystallized from a chloroform/hexanes (17:1) solution to give the title product as a yellow solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05726126uspto-grants-1998_03