2H-Imidazole, 2,2,4,5-tetrachloro- → HCID 12278431, 화합물

HRID 1973408노트

반응식

HRID 1973408 반응식
[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]

참가 물질

4

반응물 2

HCID 122783972H-Imidazole, 2,2,4,5-tetrachloro-HCID 178418546HCID 178418546, 화합물

생성물 1

HCID 12278431HCID 12278431, 화합물수율 40.2%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-fb7549e84a4649d9a78770c2ebeca11e
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03997552

반응 노트

불러오는 중…