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

HRID 746149

反応式

HRID 746149 の反応式
[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]

参加物

4

反応物 2

HCID 30177655-(2-Chloro-4-(trifluoromethyl)phenoxy)-2-nitrobenzoyl chlorideHCID 12210597HCID 12210597、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4593eaa837e64527a44451757e68ee7b
出典データセット
uspto-grants-1986_07
特許番号
US04602944

関連ノート

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