乙二胺二盐酸盐 → 乙二胺

HRID 1928

反应方程式

HRID 1928 反应方程式
[CH2:1]1[CH:6]([CH2:7][N:8]2[C:13](=[O:14])[CH:12]=[CH:11][C:9]2=[O:10])[CH2:5][CH2:4][CH:3]([C:15]([O:17][N:18]2[C:23](=[O:24])[CH:22]([S:25]([O-:28])(=[O:27])=[O:26])[CH2:21][C:19]2=[O:20])=[O:16])[CH2:2]1.[Na+:29].Cl.Cl.[CH2:32]([NH2:35])[CH2:33][NH2:34].C1C=CC(C2C(=O)C3(OC(=O)C4C3=CC=CC=4)OC=2)=CC=1>C([O-])(=O)C.[Na+]>[CH2:32]([NH2:35])[CH2:33][NH2:34].[CH2:1]1[CH:6]([CH2:7][N:8]2[C:9](=[O:10])[CH:11]=[CH:12][C:13]2=[O:14])[CH2:5][CH2:4][CH:3]([C:15]([O:17][N:18]2[C:23](=[O:24])[CH:22]([S:25]([O-:28])(=[O:27])=[O:26])[CH2:21][C:19]2=[O:20])=[O:16])[CH2:2]1.[Na+:29]

参与物

6

反应物 3

HCID 9521乙二胺二盐酸盐HCID 37927荧光胺HCID 46187944-(N-马来酰亚胺甲基)环己烷-1-羧酸磺酸基琥珀酰亚胺酯钠盐

产物 2

HCID 3301乙二胺HCID 46187944-(N-马来酰亚胺甲基)环己烷-1-羧酸磺酸基琥珀酰亚胺酯钠盐

试剂、催化剂与溶剂 1

HCID 517045醋酸钠溶剂

实验过程

Sulfo-SMCC (1 eq.)(Pierce Chemical Co., Rockford, Ill.) is dissolved in sodium acetate buffer (pH 7) and ethylenediamine dihydrochloride (5 eq.) is added. The reaction is monitored by TLC visualized with fluorescamine. When reaction is complete the reaction mixture is applied directly to a C18 reverse-phase HPLC column and eluted with a gradient of acetonitrile in triethanolamine/water, pH 7. The excess ethylene diamine elutes at the solvent front, followed by the desired product. A small amount of double coupled material formed by the condensation of one molecule of ethylenediamine with two molecules of sulfo-SMCC elutes last. The desired material is characterized by 1H NMR and IR spectroscopy, mass spectrometry, and elemental analysis.

后处理

  1. customWhen reaction
  2. washeluted with a gradient of acetonitrile in triethanolamine/water, pH 7

来源与证据

ORD记录
ord-c0cd0c63904c42eabebf3989bb71e6b3
来源数据集
uspto-grants-1998_03
专利号
US05728369

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