Chlorine → 4'-Chloro-2'-fluoroacetanilide

HRID 47004

反応式

HRID 47004 の反応式
[Cl:1]Cl.[F:3][C:4]1[CH:13]=[CH:12][CH:11]=[CH:10][C:5]=1[NH:6][C:7](=[O:9])[CH3:8]>C(O)(=O)C>[Cl:1][C:12]1[CH:11]=[CH:10][C:5]([NH:6][C:7](=[O:9])[CH3:8])=[C:4]([F:3])[CH:13]=1

参加物

4

実験手順

Seventy-one parts of liquid chlorine were added to a solution of 140 parts of 2'-fluoroacetanilide in 500 parts glacial acetic acid, during one hour, at 25°-27°, with ice water cooling. While stirring for 4 hours at 25°-27°, 4'-chloro-2'-fluoroacetanilide precipitated. After collecting the product by filtration, the filtrate was poured into 2000 parts of ice. The resulting second portion of precipitated product was collected by filtration, combined with the first portion and recrystallized from 700 parts of methanol at -45° to yield 119 parts of 4'-chloro-2'-fluoroacetanilide as white crystals melting at 152°-155°.

後処理

  1. custom4'-chloro-2'-fluoroacetanilide precipitated
  2. customAfter collecting the product
  3. filtrationby filtration
  4. additionthe filtrate was poured into 2000 parts of ice
  5. filtrationThe resulting second portion of precipitated product was collected by filtration
  6. customrecrystallized from 700 parts of methanol at -45°

出典と根拠

ORDレコード
ord-c77a75784ea749adb36e81b029d637d7
出典データセット
uspto-grants-1979_11
特許番号
US04175948

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