関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Pentylamine | HCID 8060 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-(1-Adamantyl)ethyl methanesulfonate | HCID 15717682 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(1Adamantyl)-n-pentylethylamine hydrochloride | HCID 49831680 | — |
反応手順
Pentylamine (2.69 ml, 23.2 mmol), potassium carbonate (2.14 g, 15.5 mmol) and sodium iodide (2.30 g, 15.3 mmol) were added to a solution of 2-(1-adamantyl)ethyl methanesulfonate (2.07 g, 8.01 mmol) in ethanol (45.8 ml), and the mixture was refluxed for 17 hours. The reaction mixture was concentrated under reduced pressure, and the concentrate was diluted with chloroform (100 ml). This was washed with a 1 N aqueous sodium hydroxide solution (100 ml) and a saturated aqueous sodium chloride solution (100 ml) successively, and the organic layer was dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography. A 4 N solution of hydrogen chloride in ethyl acetate (3.1 ml) was added to a solution of the resulting free form (1.52 g, 6.10 mmol) of the titled compound in ethyl acetate (0.50 ml). The precipitated solid was washed with ethyl acetate and filtered off to give 1.33 g (60%) of the titled compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07098226B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-0be30f756b24468c9c36d5c24ba0fe57 |
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| 出典メモ | uspto-grants-2006_08 |
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