2H-Imidazole, 2,2,4,5-tetrachloro- → HCID 12278431、化合物

HRID 1973408ノート

反応式

HRID 1973408 の反応式
[Cl:1][C:2]1([Cl:9])[N:6]=[C:5](Cl)[C:4]([Cl:8])=[N:3]1.[Cu][C:11]#[N:12]>C1(C)C(C)=CC=CC=1>[C:11]([C:5]1[C:4]([Cl:8])=[N:3][C:2]([Cl:1])([Cl:9])[N:6]=1)#[N:12]

参加物

4

反応物 2

HCID 122783972H-Imidazole, 2,2,4,5-tetrachloro-HCID 178418546HCID 178418546、化合物

生成物 1

HCID 12278431HCID 12278431、化合物収率 40.2%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

A mixture of 20.5 g (0.1 mol) of 2,2,4,5-tetrachloro-2H-imidazole, 41 g (0.5 mol) of anhydrous copper-(I) cyanide and 230 ml of anhydrous xylene was heated for about 30 hours at 110° - 120° C. After cooling, the reaction mixture was filtered and the brown residue was repeatedly washed with ether. The combined solutions were shaken with active charcoal and the resulting coloured solution was concentrated in vacuo. The concentrated solution was taken up in n-hexane and the product crystallised out. It was filtered off and recrystallised from n-hexane, giving 7.9 g (40% of theory) of 4-cyano-2,2,5-trichloroimidazole (melting point 114° - 115° C).

後処理

  1. temperaturewas heated for about 30 hours at 110° - 120° C
  2. temperatureAfter cooling
  3. filtrationthe reaction mixture was filtered
  4. washthe brown residue was repeatedly washed with ether
  5. concentrationthe resulting coloured solution was concentrated in vacuo
  6. customthe product crystallised out
  7. filtrationIt was filtered off
  8. customrecrystallised from n-hexane

出典と根拠

ORDレコード
ord-fb7549e84a4649d9a78770c2ebeca11e
出典データセット
uspto-grants-1976_12
特許番号
US03997552

反応ノート

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