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

HRID 1639736
ノート
印刷プレビュー

反応式

HRID 1639736 の反応式
[NH:1]1[C:9]2[CH:8]=[CH:7][CH:6]=[C:5]([C:10]([O:12][CH3:13])=[O:11])[C:4]=2[CH:3]=[N:2]1.F[B-](F)(F)F.[CH3:19][O+](C)C>C(OCC)(=O)C.C(=O)([O-])O.[Na+]>[CH3:19][N:2]1[CH:3]=[C:4]2[C:9]([CH:8]=[CH:7][CH:6]=[C:5]2[C:10]([O:12][CH3:13])=[O:11])=[N:1]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)HCID 6623327methyl 1H-indazole-4-carboxylate

生成物 1

HCID 37818684Methyl 2-methyl-2H-indazole-4-carboxylate収率 84%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒2 回HCID 516892Sodium Bicarbonate溶媒

実験手順

To a solution of methyl 1H-indazole-4-carboxylate (63.0 g, 358 mmol) in ethyl acetate (1.19 L) was added trimethyloxonium tetrafluoroborate (68.8 g, 465 mmol), and the mixture was stirred under nitrogen atmosphere at room temperature for 12 hr. The reaction solution was diluted with ethyl acetate, saturated aqueous sodium hydrogen carbonate solution was added, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by recrystallization (ethyl acetate/hexane) to give the title compound (57.0 g, yield 84%).

後処理

  1. additionwas added
  2. extractionthe mixture was extracted with ethyl acetate
  3. dry with materialThe extract was dried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by recrystallization (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-2bdca5ea3edd4eefb225ab0aef0e997b
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08110585B2

反応ノート

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