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Ethylenediamine Dihydrochloride → Ethylenediamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylenediamine Dihydrochloride | HCID 9521 | — |
| 反応物 | Fluorescamine | HCID 37927 | — |
| 反応物 | Sulfo-SMCC sodium | HCID 4618794 | — |
| 溶媒 | Sodium Acetate | HCID 517045 | — |
| 生成物 | Ethylenediamine | HCID 3301 | — |
| 生成物 | Sulfo-SMCC sodium | HCID 4618794 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05728369 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-c0cd0c63904c42eabebf3989bb71e6b3 |
| 出典メモ | uspto-grants-1998_03 |