참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Pentylamine | HCID 8060 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-(1-Adamantyl)ethyl methanesulfonate | HCID 15717682 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-(1Adamantyl)-n-pentylethylamine hydrochloride | HCID 49831680 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07098226B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-0be30f756b24468c9c36d5c24ba0fe57 |
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| 출처 메모 | uspto-grants-2006_08 |
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