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Hydrochloric Acid → N-(3,5-dichloro-2-pyridyl)-2,4-dinitro-6-trifluoromethylaniline

HRID 1065775
ノート
印刷プレビュー

反応式

HRID 1065775 の反応式
[NH2:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([Cl:9])=[CH:4][N:3]=1.[OH-].[K+].[N+:12]([C:15]1[CH:20]=[C:19]([N+:21]([O-:23])=[O:22])[CH:18]=[C:17]([C:24]([F:27])([F:26])[F:25])[C:16]=1Cl)([O-:14])=[O:13].Cl>CN(C)C=O>[Cl:8][C:7]1[C:2]([NH:1][C:16]2[C:17]([C:24]([F:26])([F:27])[F:25])=[CH:18][C:19]([N+:21]([O-:23])=[O:22])=[CH:20][C:15]=2[N+:12]([O-:14])=[O:13])=[N:3][CH:4]=[C:5]([Cl:9])[CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 67851Benzene, 2-chloro-1,5-dinitro-3-(trifluoromethyl)-HCID 778863,5-Dichloro-3-pyridylamine

生成物 1

HCID 12901603N-(3,5-dichloro-2-pyridyl)-2,4-dinitro-6-trifluoromethylaniline

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

In 20 ml. of dimethylformamide, 1.65 g. of 2-amino-3,5-dichloropyridine was dissolved and 1.0 g. of powdery potassium hydroxide was gradually added with stirring. After the addition, 2.7 g. of 2,4-dinitro-6-trifluoromethylchlorobenzene was added at 30° C. during 5 minutes to react them for about 3 hours. The reaction mixture was acidified with conc. HCl and the product was extracted with methylenechloride. 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 toluene and the solvent was distilled off to obtain 2.5 g. of the object compound having the melting point of 98° to 101° C.

後処理

  1. additionAfter the addition, 2.7 g
  2. customto react them for about 3 hours
  3. extractionthe product was extracted with methylenechloride
  4. washThe extracted layer was washed with water
  5. distillationthe solvent was distilled
  6. customThe product was separated by a silica gel column with an eluent of toluene
  7. distillationthe solvent was distilled off
  8. customto obtain 2.5 g

出典と根拠

ORDレコード
ord-043b4204da8040d5ae03f1aa5352abee
出典データセット
uspto-grants-1982_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04331670

反応ノート

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