Ethylenediamine Dihydrochloride → Ethylenediamine

HRID 1928

반응식

HRID 1928 반응식
[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]

참가 물질

6

반응물 3

HCID 9521Ethylenediamine DihydrochlorideHCID 37927FluorescamineHCID 4618794Sulfo-SMCC sodium

생성물 2

HCID 3301EthylenediamineHCID 4618794Sulfo-SMCC sodium

시약·촉매·용매 1

HCID 517045Sodium Acetate용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-c0cd0c63904c42eabebf3989bb71e6b3
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728369

연결된 노트

불러오는 중…