Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1) → HCID 59334489、化合物

HRID 1639812ノート

反応式

HRID 1639812 の反応式
[Cl:1][C:2]1[C:10]2[NH:9][N:8]=[CH:7][C:6]=2[C:5]([C:11]([O:13][CH3:14])=[O:12])=[CH:4][CH:3]=1.F[B-](F)(F)F.[CH3:20][O+](C)C>C(OCC)(=O)C.O>[Cl:1][C:2]1[C:10]2[C:6](=[CH:7][N:8]([CH3:20])[N:9]=2)[C:5]([C:11]([O:13][CH3:14])=[O:12])=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)HCID 59334582HCID 59334582、化合物

生成物 1

HCID 59334489HCID 59334489、化合物収率 71.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of methyl 7-chloro-1H-indazole-4-carboxylate (5.40 g, 25.6 mmol) in ethyl acetate (150 mL) was added trimethyloxonium tetrafluoroborate (5.69 g, 38.5 mmol) at room temperature, and the mixture was stirred for 5 hr. The is reaction solution was diluted with water, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by flash silica gel column chromatography (ethyl acetate/hexane=1/2) to give the title compound (4.10 g, yield 71%).

後処理

  1. customThe is reaction solution
  2. extractionthe mixture was extracted with ethyl acetate
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by flash silica gel column chromatography (ethyl acetate/hexane=1/2)

出典と根拠

ORDレコード
ord-c480c27de24d4275a9b467f104950681
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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