N,N-Dimethylethylenediamine → 2-(2-Dimethylamino-ethyl)-5-nitro-2H-isoquinolin-1-one

HRID 1037758ノート

反応式

HRID 1037758 の反応式
[N+:1]([C:4]1[CH:13]=[CH:12][CH:11]=[C:10]2[C:5]=1[CH:6]=[CH:7]O[C:9]2=[O:14])([O-:3])=[O:2].[CH3:15][N:16]([CH3:20])[CH2:17][CH2:18][NH2:19]>CO>[CH3:15][N:16]([CH3:20])[CH2:17][CH2:18][N:19]1[CH:7]=[CH:6][C:5]2[C:10](=[CH:11][CH:12]=[CH:13][C:4]=2[N+:1]([O-:3])=[O:2])[C:9]1=[O:14]

参加物

4

反応物 2

HCID 66053N,N-DimethylethylenediamineHCID 100127605-nitro-1H-isochromen-1-one

生成物 1

HCID 595792672-(2-Dimethylamino-ethyl)-5-nitro-2H-isoquinolin-1-one収率 46.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

5-Nitro-isochromen-1-one (1.0 g, 5.2 mmol) and N,N-dimethyl-1,2-ethanediamine (4 g, 40 mmol) were refluxed in methanol (40 mL) for 1.5 hours. The volatiles were removed via rotovapor and the residue was purified via flash chromatography (12 of silica gel, 0-70% EtOAc/CH2Cl2 gradient) gave 2-(2-Dimethylamino-ethyl)-5-nitro-2H-isoquinolin-1-one as a yellow solid (1.4 g, 2.4 mmol, 46%).

後処理

  1. customThe volatiles were removed via rotovapor
  2. customthe residue was purified via flash chromatography (12 of silica gel, 0-70% EtOAc/CH2Cl2 gradient)

出典と根拠

ORDレコード
ord-ad5007f8d2c24f1c87404450cb50a61b
出典データセット
uspto-grants-2013_10
特許番号
US08546579B2

反応ノート

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