N-bromobutanimide → HCID 178497388, 화합물

HRID 503183노트

반응식

HRID 503183 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178497388HCID 178497388, 화합물수율 97%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2908cb1328124f0cb2c8eb9705db838d
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776890B2

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