Imidazole → 3-Chloro-6-(1H-imidazol-1-yl)pyridazine

HRID 359418노트

반응식

HRID 359418 반응식
[NH:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.[H-].[Na+].[Cl:8][C:9]1[N:10]=[N:11][C:12](Cl)=[CH:13][CH:14]=1>CN(C)C=O>[Cl:8][C:9]1[N:10]=[N:11][C:12]([N:1]2[CH:5]=[CH:4][N:3]=[CH:2]2)=[CH:13][CH:14]=1

참가 물질

5

반응물 3

HCID 795ImidazoleHCID 24758Sodium hydrideHCID 673313,6-Dichloropyridazine

생성물 1

HCID 27709033-Chloro-6-(1H-imidazol-1-yl)pyridazine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

A mixture of 47.6 parts of 1H-imidazole, 33.6 parts of sodium hydride dispersion 50% and 750 parts of N,N-dimethylformamide was stirred at room temperature for 15 minutes. The resulting solution was added to 106 parts of 3,6-dichloropyridazine in 750 parts of N,N-dimethylformamide and the whole was further stirred for 2 days at room temperature. The product was extracted with trichloromethane. The extract was dried, filtered and evaporated. The residue was crystallized from methanol. The product was filtered off, washed with petroleumether and dried, yielding 48.5 parts of 3-chloro-6-(1H-imidazol-1-yl)pyridazine; mp. 182.9° C. (compound 1).

후처리

  1. stirringthe whole was further stirred for 2 days at room temperature
  2. extractionThe product was extracted with trichloromethane
  3. customThe extract was dried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was crystallized from methanol
  7. filtrationThe product was filtered off
  8. washwashed with petroleumether
  9. customdried

출처 및 근거

ORD 기록
ord-3d4d7ddcce3a484388e305124e2ac8dd
출처 데이터셋
uspto-grants-1991_03
특허 번호
US05001125

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