関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylenetetramine | HCID 5565 | — |
| 反応物 | Oleoyl chloride | HCID 5364783 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | Trientine HCl | HCID 5458180 | — |
反応手順
1.12 g (7.5 mmol) of triethylenetetramine was added to 25 mL of dichloromethane and dissolved with stirring in an ice water bath at 5° C. for 30 minutes. To the solution, a solution of 2.00 g (6.0 mmol) of oleoyl chloride in 20 mL of dichloromethane in a separate reactor was added slowly dropwise while it was allowed to react at 5° C. for 3 hours. Due to hydrogen chloride produced during the reaction, unreacted triethylenetetramine HCl was precipitated. Before the end of the reaction, the upper layer solution was taken and analyzed by thin layer chromatography (TLC) with a mobile phase of ethanol:chloroform (2:1) to determine whether the reaction was completed. After it was determined that the reaction had completed, the precipitate was removed using filter paper.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09220779B2 |
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| 出典データセット | uspto-grants-2015_12 |
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| ORD ID | ord-f91ac25f048145769fee06a6a5f93ca5 |
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| 出典メモ | uspto-grants-2015_12 |
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