Acetic Acid → 8-Bromo-1-methyl-[1,2,4]triazolo[4,3-a]quinoxaline

HRID 711384노트

반응식

HRID 711384 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:14](O)(=O)[CH3:15]>>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[CH:7][C:8]3[N:9]2[C:14]([CH3:15])=[N:13][N:12]=3)=[CH:4][CH:3]=1

참가 물질

3

반응물 2

HCID 176Acetic AcidHCID 52002657-Bromo-2-hydrazinylquinoxaline

생성물 1

HCID 668035548-Bromo-1-methyl-[1,2,4]triazolo[4,3-a]quinoxaline수율 90%

실험 절차

A mixture of 7-bromo-2-hydrazinylquinoxaline (1 g, 4.18 mmol) in acetic acid (10 mL) was refluxed for 18 h. Half of the acetic acid was removed under vacuum and the residue was poured into ice-water. The precipitate was collected on a filter, washed with water, and dried under vacuo to afford crude 8-bromo-1-methyl-[1,2,4]triazolo[4,3-a]quinoxaline as a dark red solid (1 g, yield 90%) which was used in the next step without further purification. MS (m/z): 263 (M+H)+.

후처리

  1. temperaturewas refluxed for 18 h
  2. customHalf of the acetic acid was removed under vacuum
  3. additionthe residue was poured into ice-water
  4. customThe precipitate was collected on a filter
  5. washwashed with water
  6. customdried under vacuo

출처 및 근거

ORD 기록
ord-5d14d82332fb4e68aafe04a1a681c519
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181264B2

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