3-(2,6-Dichloro-4-trifluoromethylphenylhydrazino)propionitrile → HCID 21982150、化合物

HRID 10766ノート

反応式

HRID 10766 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[NH:13][NH:14][CH2:15][CH2:16][C:17]#[N:18]>ClC1C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:10])([F:9])[F:11])[CH:5]=[C:4]([Cl:12])[C:3]=1[NH:13][N:14]=[CH:15][CH2:16][C:17]#[N:18].[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:10])([F:9])[F:11])[CH:5]=[C:4]([Cl:12])[C:3]=1[N:13]=[N:14][CH2:15][CH2:16][C:17]#[N:18]

参加物

4

反応物 1

HCID 110878053-(2,6-Dichloro-4-trifluoromethylphenylhydrazino)propionitrile

生成物 2

HCID 21982150HCID 21982150、化合物HCID 695517003-{2-[2,6-Dichloro-4-(trifluoromethyl)phenyl]hydrazinylidene}propanenitrile

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

反応条件

温度
65 °C

実験手順

Cupric chloride (0.673 g, 2.5 equivalents) was added in one portion to a solution of 3-(2,6-dichloro-4-trifluoromethylphenylhydrazino)propionitrile (0.591 g, 2 mmol) in chlorobenzene, and the mixture heated at 65° C. for 50 minutes. The reaction was judged to be complete and was cooled, washed (water), dried (magnesium sulfate), evaporated and separated by chromatography on silica gel to give 3-(2,6-dichloro-4-trifluoromethylphenylhydrazono)propionitrile, NMR 3.37 (d, 2H), 7.03 (t, 1H), 7.5 (s, 2H), 7.75 (s, 1H) (35% yield), and 3-(2,6-dichloro-4trifluoromethylphenylazo)propionitrile, NMR 3.0 (t, 2H), 4.6 (t, 2H), 7.6 (s, 2H) (60% yield).

後処理

  1. temperaturewas cooled
  2. washwashed (water)
  3. dry with materialdried (magnesium sulfate)
  4. customevaporated
  5. customseparated by chromatography on silica gel

出典と根拠

ORDレコード
ord-51889edae8a3452c876a139b2f003a44
出典データセット
uspto-grants-2006_08
特許番号
US07094906B2

反応ノート

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