Stannous Chloride → 5-Amino-2-(2-dimethylamino-ethyl)-2H-isoquinolin-1-one

HRID 1037759ノート

反応式

HRID 1037759 の反応式
[CH3:1][N:2]([CH3:19])[CH2:3][CH2:4][N:5]1[CH:14]=[CH:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[N+:15]([O-])=O)[C:6]1=[O:18].[Sn](Cl)Cl>C1COCC1>[NH2:15][C:11]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:12]=1[CH:13]=[CH:14][N:5]([CH2:4][CH2:3][N:2]([CH3:19])[CH3:1])[C:6]2=[O:18]

参加物

4

反応物 2

HCID 24479Stannous ChlorideHCID 595792672-(2-Dimethylamino-ethyl)-5-nitro-2H-isoquinolin-1-one

生成物 1

HCID 595794535-Amino-2-(2-dimethylamino-ethyl)-2H-isoquinolin-1-one

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

2-(2-Dimethylamino-ethyl)-5-nitro-2H-isoquinolin-1-one (0.67 g, 2.6 mmol) and dehydrate tin dichloride (2 g, 10 mml) were stirred in THF (10 mL) at room temperature for 24 hours. The volatiles were removed via rotovapor, and the residue was dissolved in CH2Cl2 (1 L), washed with aqueous saturated NaHCO3 solution (30 mL×3). The organic layer was dried over Na2SO4, filtered and concentrated to dryness gave 5-Amino-2-(2-dimethylamino-ethyl)-2H-isoquinolin-1-one as a yellow solid. The compound was used for next steps without further purification.

後処理

  1. customThe volatiles were removed via rotovapor
  2. dissolutionthe residue was dissolved in CH2Cl2 (1 L)
  3. washwashed with aqueous saturated NaHCO3 solution (30 mL×3)
  4. dry with materialThe organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-b77dc1712f8e4d5ca9009d9e2cc01e18
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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