Chlorine → 4'-Chloro-2'-fluoroacetanilide

HRID 1076920

反応式

HRID 1076920 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

反応物 2

HCID 24526ChlorineHCID 67860N-(2-Fluorophenyl)acetamide

生成物 1

HCID 8531744'-Chloro-2'-fluoroacetanilide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

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°C, with icewater cooling. While stirring for 4 hours at 25°-27°C, 4'-chloro-2'-fluoroacetanilide precipitated. After collecting the product by filtration, the filtrate was poured over 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°C to yield 119 parts of 4'-chloro-2'-fluoroacetanilide as white crystals melting at 152°-155°C.

後処理

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

出典と根拠

ORDレコード
ord-77dfad2de8d049b7846f5ef1b3d80755
出典データセット
uspto-grants-1976_05
特許番号
US03958976

関連ノート

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