Nitric Acid → N-(5-chloro-4-fluoro-2-nitrophenyl)acetamide

HRID 1761641노트

반응식

HRID 1761641 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10](=[O:12])[CH3:11])[CH:5]=[CH:6][C:7]=1[F:8].[N+:13]([O-])([OH:15])=[O:14]>S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10](=[O:12])[CH3:11])[C:5]([N+:13]([O-:15])=[O:14])=[CH:6][C:7]=1[F:8]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 589188N-(3-Chloro-4-fluorophenyl)acetamide

생성물 1

HCID 2773811N-(5-chloro-4-fluoro-2-nitrophenyl)acetamide

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

To a solution of N-(3-chloro-4-fluorophenyl)acetamide (55 g) in concentrated sulfuric acid (165 ml) was added dropwise concentrated nitric acid (d 1.42, 154 ml) at 5°-10° C. during an hour with stirring in an ice-salt bath. After stirring for an hour at the same temperature, the reaction mixture was poured into ice water. The resulting precipitate was collected by filtration, sufficiently washed with water and recrystallized from acetonitrile to give the title compound (48.9 g) as yellow needles, mp 114°-115° C.

후처리

  1. stirringAfter stirring for an hour at the same temperature
  2. filtrationThe resulting precipitate was collected by filtration
  3. washsufficiently washed with water
  4. customrecrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-9e29a83732db4959a8020002b024b850
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04826982

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