Dimethyl Sulfoxide → 2-Pyridinamine, 3-chloro-N-(3-ethoxy-2,6-dinitro-4-(trifluoromethyl)phenyl)-5-(trifluoromethyl)-

HRID 1065780ノート

反応式

HRID 1065780 の反応式
[CH2:1]([OH:3])[CH3:2].[H-].[Na+].[Cl:6][C:7]1[C:8]([NH:17][C:18]2[C:23]([N+:24]([O-:26])=[O:25])=[CH:22][C:21]([C:27]([F:30])([F:29])[F:28])=[C:20](Cl)[C:19]=2[N+:32]([O-:34])=O)=[N:9][CH:10]=[C:11]([C:13]([F:16])([F:15])[F:14])[CH:12]=1.CS(C)=O.[OH2:39]>>[Cl:6][C:7]1[C:8]([NH:17][C:18]2[C:19]([N+:32]([O-:34])=[O:39])=[CH:20][C:21]([C:27]([F:30])([F:28])[F:29])=[C:22]([O:3][CH2:1][CH3:2])[C:23]=2[N+:24]([O-:26])=[O:25])=[N:9][CH:10]=[C:11]([C:13]([F:14])([F:15])[F:16])[CH:12]=1

参加物

6

反応物 5

HCID 679Dimethyl SulfoxideHCID 702EthanolHCID 962WaterHCID 24758Sodium hydrideHCID 91731Fluazinam

生成物 1

HCID 1575522-Pyridinamine, 3-chloro-N-(3-ethoxy-2,6-dinitro-4-(trifluoromethyl)phenyl)-5-(trifluoromethyl)-

実験手順

In 30 ml. of ethanol, 1.5 g. of sodium hydride was added with stirring and a solution of 7.0 g. of N-(3-chloro-5-trifluoromethyl-2-pyridyl)-2,6-dinitro-3-chloro-4-trifluoromethylaniline (obtained in Preparation 4) in 50 ml. of dimethylsulfoxide was added dropwise to react them at room temperature for 3 hours. The reaction mixture was poured into water and the product was extracted with methylene chloride. The extracted layer was washed with water and dehydrated and the solvent was distilled, the product was separated by a silica gel column with an eluent of a mixture of n-hexane and ethyl acetate (4:1) and the solvent was distilled off to obtain 4.0 g. of the object compound having the melting point of 106° to 108° C.

後処理

  1. customto react them at room temperature for 3 hours
  2. extractionthe product was extracted with methylene chloride
  3. washThe extracted layer was washed with water
  4. distillationthe solvent was distilled
  5. customthe product was separated by a silica gel column with an eluent of a mixture of n-hexane and ethyl acetate (4:1)
  6. distillationthe solvent was distilled off
  7. customto obtain 4.0 g

出典と根拠

ORDレコード
ord-203d99bc989f40ebbbb4e923df10f59d
出典データセット
uspto-grants-1982_05
特許番号
US04331670

反応ノート

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