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

HRID 711384ノート

反応式

HRID 711384 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: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

参加物

3

反応物 2

HCID 176Acetic AcidHCID 52002657-Bromo-2-hydrazinylquinoxaline

生成物 1

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

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-5d14d82332fb4e68aafe04a1a681c519
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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