Triethylamine → 8-bromo-[1,2,4]triazolo[4,3-a]quinoxalin-1(2H)-one

HRID 711368ノート

反応式

HRID 711368 の反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[CH:7][C:8]([NH:12][NH2:13])=[N:9]2)=[CH:4][CH:3]=1.C(N(CC)CC)C.[O:21]=[C:22](Cl)OC(Cl)(Cl)Cl>ClCCl>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[CH:7][C:8]3[N:9]2[C:22](=[O:21])[NH:13][N:12]=3)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10426DiphosgeneHCID 52002657-Bromo-2-hydrazinylquinoxaline

生成物 1

HCID 668030988-bromo-[1,2,4]triazolo[4,3-a]quinoxalin-1(2H)-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To the solution of 7-bromo-2-hydrazinylquinoxaline (200 mg, 0.83 mmol) in dichloromethane (5 mL) was added triethylamine (0.175 mL, 1.2 mmol), then the solution of diphosgene (0.055 mL, 0.46 mmol) in dichloromethane was added dropwise at 0° C. with stirring under nitrogen atmosphere. After stirring at r.t. for 5 h, the solvent was removed under vacuum, the residue was washed with water, and dried in vacuo to afford the title product 8-bromo-[1,2,4]triazolo[4,3-a]quinoxalin-1(2H)-one as yellow solid in 82% yield (180 mg). m/z 265 (M+H)+.

後処理

  1. stirringAfter stirring at r.t. for 5 h
  2. customthe solvent was removed under vacuum
  3. washthe residue was washed with water
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-84a79d67dcf54646bf5417f0a12d5ace
出典データセット
uspto-grants-2015_11
特許番号
US09181264B2

反応ノート

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