N-bromobutanimide → 3-Bromo-6-difluoromethoxy-2-(3-fluoro-phenyl)-pyrazolo[1,5-b]pyridazine

HRID 1280414노트

반응식

HRID 1280414 반응식
[Br:1]N1C(=O)CCC1=O.[F:9][CH:10]([F:28])[O:11][C:12]1[CH:13]=[CH:14][C:15]2[N:16]([N:18]=[C:19]([C:21]3[CH:26]=[CH:25][CH:24]=[C:23]([F:27])[CH:22]=3)[CH:20]=2)[N:17]=1.C(=O)(O)[O-].[Na+]>CN(C=O)C.C(OCC)(=O)C>[Br:1][C:20]1[C:19]([C:21]2[CH:26]=[CH:25][CH:24]=[C:23]([F:27])[CH:22]=2)=[N:18][N:16]2[C:15]=1[CH:14]=[CH:13][C:12]([O:11][CH:10]([F:9])[F:28])=[N:17]2

참가 물질

6

반응물 3

HCID 67184N-bromobutanimideHCID 516892Sodium BicarbonateHCID 225623316-Difluoromethoxy-2-(3-fluoro-phenyl)-pyrazolo[1,5-b]pyridazine

생성물 1

HCID 225623333-Bromo-6-difluoromethoxy-2-(3-fluoro-phenyl)-pyrazolo[1,5-b]pyridazine수율 91%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

N-bromo succinimide (195 mg) was added to a solution of 6-difluoromethoxy-2-(3-fluoro-phenyl)-pyrazolo[1,5-b]pyridazine (251 mg) and sodium bicarbonate (185 mg) in anhydrous DMF (10 ml) and stirred for 18 h. The reaction mixture was diluted with ethyl acetate (300 ml) and washed with water (10×20 ml), brine (20 ml), dried (Na2SO4) and concentrated to give the title compound as a solid (293 mg, 91%).

후처리

  1. washwashed with water (10×20 ml), brine (20 ml)
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-45985f9b5cdb4445aca3687c08183b57
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06451794B1

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