三乙胺 → 8-bromo-[1,2,4]triazolo[4,3-a]quinoxalin-1(2H)-one

HRID 711368笔记

反应方程式

HRID 711368 反应方程式
[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

参与物

5

反应物 3

HCID 8471三乙胺HCID 10426氯甲酸三氯甲酯HCID 52002657-Bromo-2-hydrazinylquinoxaline

产物 1

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

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂2 次

实验过程

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)+.

后处理

  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

来源与证据

ORD记录
ord-84a79d67dcf54646bf5417f0a12d5ace
来源数据集
uspto-grants-2015_11
专利号
US09181264B2

反应笔记

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