1,4-Cyclohexanedimethanamine → N'-[4-(aminomethyl)cyclohexyl]methyl-N,N-dimethylsulfamide

HRID 413663

反応式

HRID 413663 の反応式
[CH3:1][N:2]([CH3:7])[S:3](Cl)(=[O:5])=[O:4].[NH2:8][CH2:9][CH:10]1[CH2:15][CH2:14][CH:13]([CH2:16][NH2:17])[CH2:12][CH2:11]1.C(N(C(C)C)CC)(C)C>ClCCl>[NH2:8][CH2:9][CH:10]1[CH2:15][CH2:14][CH:13]([CH2:16][NH:17][S:3]([N:2]([CH3:7])[CH3:1])(=[O:5])=[O:4])[CH2:12][CH2:11]1

参加物

5

反応物 3

HCID 173541,4-CyclohexanedimethanamineHCID 81531DiisopropylethylamineHCID 83372Dimethylsulphamoyl chloride

生成物 1

HCID 22254077N'-[4-(aminomethyl)cyclohexyl]methyl-N,N-dimethylsulfamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Dimethylsulfamoyl chloride (one mol-equivalent, ClSO2N(CH3)2) was added to a stirred solution of 1,4-bis-aminomethylcyclohexane (3 mol-equivalents) and diisopropylethylamine (1 mol-equivalent) in dichloromethane at 0° C. The reaction mixture was stirred at room temperature for 24 hours, concentrated under reduced pressure and chromatographed (silica) to give the desired product as viscous oils. (Scheme 1A)

後処理

  1. concentrationconcentrated under reduced pressure
  2. customchromatographed (silica)

出典と根拠

ORDレコード
ord-1c4980a30bde4d3e8e831941d46524ea
出典データセット
uspto-grants-2003_05
特許番号
US06569856B2

関連ノート

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