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

HRID 711368노트

반응식

HRID 711368 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-84a79d67dcf54646bf5417f0a12d5ace
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181264B2

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