Difluoroacetic acid → 6-Chloro-3-(difluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazine

HRID 1674760

반응식

HRID 1674760 반응식
[Cl:1][C:2]1[N:3]=[N:4][C:5]([NH:8][NH2:9])=[CH:6][CH:7]=1.[F:10][CH:11]([F:15])[C:12](O)=O>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]2[N:4]([C:12]([CH:11]([F:15])[F:10])=[N:9][N:8]=2)[N:3]=1

참가 물질

3

반응물 2

HCID 9788Difluoroacetic acidHCID 1007873-Chloro-6-hydrazinopyridazine

생성물 1

HCID 14723856-Chloro-3-(difluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazine수율 84.7%

반응 조건

온도
100 °C

실험 절차

A mixture of 3-chloropyridazin-6-yl hydrazine (5.0 g, 34.72 mmol) and difluoroacetic acid (21.93 mL; ca. 347 mmol) was heated at 100° C. for 3 hours and then evaporated to dryness. The involatile residue was dissolved in ethyl acetate (200 mL) and washed sequentially with saturated aqueous sodium carbonate and then saturated brine. The organic phase was dried over MgSO4, filtered, and evaporated to give 6-chloro-3-difluoromethyl-[1,2,4]-triazolo[4,3-b]pyridazine (6.0 g, 84.7%) as a white solid that was used without further purification.

후처리

  1. customevaporated to dryness
  2. dissolutionThe involatile residue was dissolved in ethyl acetate (200 mL)
  3. washwashed sequentially with saturated aqueous sodium carbonate
  4. dry with materialThe organic phase was dried over MgSO4
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-0ceaf4b1da1f4d33957a3227a815b9d9
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08003649B2

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