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Sodium Hydroxide → 2-(2-Dimethylaminobenzylthio)quinoxaline

HRID 2107325
ノート
印刷プレビュー

反応式

HRID 2107325 の反応式
[SH:1][C:2]1[CH:11]=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[OH-].[Na+].Cl.[CH3:15][N:16]([CH3:25])[C:17]1[CH:24]=[CH:23][CH:22]=[CH:21][C:18]=1[CH2:19]Cl>C(O)C.O>[CH3:15][N:16]([CH3:25])[C:17]1[CH:24]=[CH:23][CH:22]=[CH:21][C:18]=1[CH2:19][S:1][C:2]1[CH:11]=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 135374262-(chloromethyl)-N,N-dimethylaniline hydrochlorideHCID 178418602HCID 178418602、化合物

生成物 1

HCID 140521762-(2-Dimethylaminobenzylthio)quinoxaline収率 82.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water
溶媒

実験手順

To a solution of 1 g of 2-mercaptoquinoxaline in 40 ml of ethanol was added a solution of 530 mg of sodium hydroxide in 2 ml of water, and subsequently added 1.27 g of 2-dimethylaminobenzyl chloride hydrochloride. The resulting mixture was stirred at room temperature for 18 hrs., and the solvent was removed under reduced pressure. The residue was extracted with ethyl acetate. The organic layer was washed successively with 5% aqueous sodium hydroxide solution, water, and saturated aqueous sodium chloride solution, and dried over soidum sulfate. The sodium sulfate was removed by filtration, and the filtrate was placed under reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography (hexane/acetone) to give 1.5 g of 2-(2-dimethylaminobenzylthio)quinoxaline as a yellow oil.

後処理

  1. custom, and the solvent was removed under reduced pressure
  2. extractionThe residue was extracted with ethyl acetate
  3. washThe organic layer was washed successively with 5% aqueous sodium hydroxide solution, water, and saturated aqueous sodium chloride solution
  4. dry with materialdried over soidum sulfate
  5. customThe sodium sulfate was removed by filtration
  6. customto remove the solvent
  7. customThe residue was purified by silica gel column chromatography (hexane/acetone)

出典と根拠

ORDレコード
ord-e4eb99e92814483f83cf7794b38a878e
出典データセット
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04933458

反応ノート

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