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

HRID 1639763ノート

反応式

HRID 1639763 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 225590314-Bromo-2-methyl-2H-indazole収率 95.2%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-c01811fb97ed44e7b82c931aae8cf18b
出典データセット
uspto-grants-2012_02
特許番号
US08110585B2

反応ノート

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