5-(((2-Aminoethyl)thio)methyl)-N,N-dimethyl-2-furanmethanamine → 3-{2-[(5-Dimethylaminomethyl-2-furyl)methylthio]ethylamino}-4-(3-pyridyl)methylamino-1,2,5-thiadiazole 1-oxide

HRID 2418120ノート

反応式

HRID 2418120 の反応式
CO[C:3]1[C:7]([NH:8][CH2:9][C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)=[N:6][S:5](=[O:16])[N:4]=1.[CH3:17][N:18]([CH2:20][C:21]1[O:25][C:24]([CH2:26][S:27][CH2:28][CH2:29][NH2:30])=[CH:23][CH:22]=1)[CH3:19]>CO>[CH3:19][N:18]([CH2:20][C:21]1[O:25][C:24]([CH2:26][S:27][CH2:28][CH2:29][NH:30][C:3]2[C:7]([NH:8][CH2:9][C:10]3[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=3)=[N:6][S:5](=[O:16])[N:4]=2)=[CH:23][CH:22]=1)[CH3:17]

参加物

4

反応物 2

HCID 1622035-(((2-Aminoethyl)thio)methyl)-N,N-dimethyl-2-furanmethanamineHCID 204020453-Methoxy-4-(3-pyridyl)methylamino-1,2,5-thiadiazole 1-oxide

生成物 1

HCID 159641483-{2-[(5-Dimethylaminomethyl-2-furyl)methylthio]ethylamino}-4-(3-pyridyl)methylamino-1,2,5-thiadiazole 1-oxide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To the methanol solution of 3-methoxy-4-(3-pyridyl)methylamino-1,2,5-thiadiazole 1-oxide produced in Step A was added a solution of 2-[(5-dimethylaminomethyl-2-furyl)methylthio]ethylamine (4.0 g; 18.7 mmoles) in 30 ml of methanol. The reaction mixture was stirred at ambient temperatures for 18 hours and the solvent was removed in vacuo. The residue was placed on 500 g of silica gel (230-400 mesh) and purified by flash chromatography using a gradient elution of acetonitrile-methanol. After combining the appropriate fractions, the title compound was obtained as an amber oil (4.25 g) containing one mole of methanol.

後処理

  1. customthe solvent was removed in vacuo
  2. custompurified by flash chromatography
  3. washa gradient elution of acetonitrile-methanol

出典と根拠

ORDレコード
ord-d8a12b780c30441490d3e97e6e18b140
出典データセット
uspto-grants-1984_09
特許番号
US04471122

反応ノート

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