Chlorine → 4'-Chloro-2'-fluoroacetanilide

HRID 441693

반응식

HRID 441693 반응식
[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

참가 물질

4

실험 절차

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 ice-water 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.

후처리

  1. custom4'-chloro-2'-fluoroacetanilide precipitated
  2. customAfter collecting the product
  3. filtrationby filtration
  4. additionthe filtrate was poured over 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° C.

출처 및 근거

ORD 기록
ord-568b5c017eaf452d907981e821a347a1
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04042373

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