N,N-Dimethylethylenediamine → N'-(6,7-Dichloro-3-pyridin-2-yl-quinoxalin-2-yl)-N,N-dimethyl-ethane-1,2-diamine

HRID 1266139ノート

反応式

HRID 1266139 の反応式
Cl[C:2]1[C:11]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=2)=[N:10][C:9]2[C:4](=[CH:5][C:6]([Cl:19])=[C:7]([Cl:18])[CH:8]=2)[N:3]=1.[CH3:20][N:21]([CH3:25])[CH2:22][CH2:23][NH2:24]>C1(C)C=CC=CC=1>[Cl:18][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][C:6]=1[Cl:19])[N:3]=[C:2]([NH:24][CH2:23][CH2:22][N:21]([CH3:25])[CH3:20])[C:11]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=1)=[N:10]2

参加物

4

反応物 2

HCID 66053N,N-DimethylethylenediamineHCID 185490312,6,7-Trichloro-3-pyridin-2-yl-quinoxaline

生成物 1

HCID 9906985N'-(6,7-Dichloro-3-pyridin-2-yl-quinoxalin-2-yl)-N,N-dimethyl-ethane-1,2-diamine収率 44.6%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 2,6,7-trichloro-3-pyridin-2-yl-quinoxaline (0.50 g) and N,N-dimethyl-ethane-1,2-diamine (0.28 g) in toluene (20 mL) was refluxed under nitrogen atmosphere for 16 hours. After refluxing, the reaction mixture was cooled, filtered, and concentrated under vacuum. The residue was purified by flash chromatography (silica gel, 1:9 methanol/dichloromethane) to give the product as a yellow solid (0.26 g); mp 95-97° C.

後処理

  1. temperatureAfter refluxing
  2. temperaturethe reaction mixture was cooled
  3. filtrationfiltered
  4. concentrationconcentrated under vacuum
  5. customThe residue was purified by flash chromatography (silica gel, 1:9 methanol/dichloromethane)

出典と根拠

ORDレコード
ord-c5c5f204f6d14b77aa5808ca7327407c
出典データセット
uspto-grants-2003_04
特許番号
US06548499B1

反応ノート

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