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

HRID 457675

反応式

HRID 457675 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-5e70ce1d4c6c492c8f28d8f2334634c4
出典データセット
uspto-grants-2007_03
特許番号
US07189720B2

関連ノート

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