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4-Fluorobenzonitrile → HCID 178509531、化合物

HRID 503110
ノート
印刷プレビュー

反応式

HRID 503110 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([C:10]#[N:11])=[CH:7][CH:8]=2)[CH:3]=[N:2]1.FC1C=CC(C#N)=CC=1.[Br:21]N1C(=O)CCC1=O>CN(C)C=O>[Br:21][C:3]1[C:4]2[C:9](=[CH:8][CH:7]=[C:6]([C:10]#[N:11])[CH:5]=2)[NH:1][N:2]=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 3

HCID 145174-FluorobenzonitrileHCID 67184N-bromobutanimideHCID 111263841H-Indazole-5-carbonitrile

生成物 1

HCID 178509531HCID 178509531、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 300 mg of a compound 1H-5-indazolecarbonitrile (synthesized from 4-fluorobenzonitrile according to the procedures described in literature, Tetrahedron Lett., 33, 7499 (1992) and Synthetic commun., 27, 1199 (1997)) in 3 ml dimethylformamide was added 392 mg of N-bromosuccinimide at room temperature, and the mixture was stirred at the same temperature for one day. After removing the solvent by distillation, the residue was added with 25 ml of ethyl acetate. 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 440 mg of the title compound as pale red crystals.

後処理

  1. customAfter removing the solvent
  2. distillationby distillation
  3. additionthe residue was added with 25 ml of ethyl acetate
  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-3c41e472df1242bfb89a701dda4f1773
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07776890B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート