N-bromobutanimide → HCID 178497388、化合物

HRID 1610140ノート

反応式

HRID 1610140 の反応式
[CH3:1][O:2][C:3]([C:5]1[C:6]([F:14])=[C:7]2[C:11](=[CH:12][CH:13]=1)[NH:10][N:9]=[CH:8]2)=[O:4].[Br:15]N1C(=O)CCC1=O>CN(C)C=O>[CH3:1][O:2][C:3]([C:5]1[C:6]([F:14])=[C:7]2[C:11](=[CH:12][CH:13]=1)[NH:10][N:9]=[C:8]2[Br:15])=[O:4]

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 59797108methyl 4-fluoro-1H-indazole-5-carboxylate

生成物 1

HCID 178497388HCID 178497388、化合物収率 97%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2.2 g of 4-fluoro-1H-5-indazolecarboxylic acid methyl ester obtained in Production Example II-13-c in 20 ml dimethylformamide was added 2.12 g of N-bromosuccinimide at room temperature, and the mixture was stirred at the same temperature for 1 hour. After removing the solvent by distillation, 120 ml of ethyl acetate was added to the residue. The mixture was sequentially washed with half-saturated aqueous sodium hydrogencarbonate solution, water and brine, dried over anhydrous magnesium sulfate and the solvent was evaporated, to give 3.0 g of the title compound as bright yellow crystals.

後処理

  1. customAfter removing the solvent
  2. distillationby distillation, 120 ml of ethyl acetate
  3. additionwas added to the residue
  4. washThe mixture was sequentially washed with half-saturated aqueous sodium hydrogencarbonate solution, water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-b78531d3783745f08bcdaccbf9e2fbe7
出典データセット
uspto-grants-2006_01
特許番号
US06982274B2

反応ノート

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