Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1) → 4-Bromo-2-methyl-2H-indazole

HRID 1639763노트

반응식

HRID 1639763 반응식
[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[N:5][NH:6]2.F[B-](F)(F)F.[CH3:16][O+](C)C>C(OCC)(=O)C>[Br:1][C:2]1[C:3]2[C:7]([CH:8]=[CH:9][CH:10]=1)=[N:6][N:5]([CH3:16])[CH:4]=2

참가 물질

4

반응물 2

HCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)HCID 223525484-bromo-1H-indazole

생성물 1

HCID 225590314-Bromo-2-methyl-2H-indazole수율 95.2%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

To a solution of 4-bromo-1H-indazole (2.24 g, 11.4 mmol) in ethyl acetate (110 mL) was added trimethyloxonium tetrafluoroborate (2.19 g, 14.8 mmol) at room temperature, and the mixture was stirred for 3 hr. The reaction solution was diluted with ethyl acetate, washed with aqueous sodium hydrogen carbonate solution and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane=10/90→40/60) to give the title compound (2.29 g, yield 95%).

후처리

  1. washwashed with aqueous sodium hydrogen carbonate solution
  2. dry with materialdried over anhydrous sodium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane=10/90→40/60)

출처 및 근거

ORD 기록
ord-c01811fb97ed44e7b82c931aae8cf18b
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08110585B2

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