5-(2-Chloro-4-(trifluoromethyl)phenoxy)-2-nitrobenzoyl chloride → 1-[5-(2-Chloro-4-trifluoromethylphenoxy)-2-nitrobenzamido]pyridinium chloride

HRID 746149

반응식

HRID 746149 반응식
[Cl-].[NH2:2][N+:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[Cl:9][C:10]1[CH:28]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:26]=[CH:25][C:11]=1[O:12][C:13]1[CH:14]=[CH:15][C:16]([N+:22]([O-:24])=[O:23])=[C:17]([CH:21]=1)[C:18](Cl)=[O:19]>C(#N)C>[Cl-:9].[Cl:9][C:10]1[CH:28]=[C:27]([C:29]([F:30])([F:32])[F:31])[CH:26]=[CH:25][C:11]=1[O:12][C:13]1[CH:14]=[CH:15][C:16]([N+:22]([O-:24])=[O:23])=[C:17]([CH:21]=1)[C:18]([NH:2][N+:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)=[O:19]

참가 물질

4

반응물 2

HCID 30177655-(2-Chloro-4-(trifluoromethyl)phenoxy)-2-nitrobenzoyl chlorideHCID 12210597HCID 12210597, 화합물

생성물 1

HCID 202407781-[5-(2-Chloro-4-trifluoromethylphenoxy)-2-nitrobenzamido]pyridinium chloride수율 156.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

1-Aminopyridinium chloride (2.9 g) was added to 5-(2-chloro-4-trifluoromethylphenoxy)-2-nitrobenzoyl chloride (7.6 g) in acetonitrile (50 ml). The mixture was stirred and heated to reflux. After 20 minutes a solid precipitated. Reflux was continued for a further 40 minutes. Then the mixture was cooled in ice and the solid filtered off. The solid was washed with cold acetonitrile, then with ether, and was air dried to give 7.4 g of the desired product, mp 234°-237° C.

후처리

  1. temperatureheated to reflux
  2. customAfter 20 minutes a solid precipitated
  3. temperatureReflux
  4. temperatureThen the mixture was cooled in ice
  5. filtrationthe solid filtered off
  6. washThe solid was washed with cold acetonitrile
  7. customdried

출처 및 근거

ORD 기록
ord-4593eaa837e64527a44451757e68ee7b
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04602944

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