참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Isonicotinic Acid | HCID 5922 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | 4-[4-(2-tert-Butyl-6-cyclobutyl-pyrimidin-4-yl)piperazin-1-yl]-butylamine | HCID 69026067 | — |
| 반응물 | HCID 178418300 | HCID 178418300 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 69078470 | HCID 69078470 | 72.3% |
반응 단계
0.35 g of isonicotinic acid (2.84 mmol) and 0.87 g of triethylamine (8.62 mmol) were dissolved in 30 ml of dimethylformamide. 0.45 g of hydroxybenzotriazole (HOBt, 3.33 mmol), 1.1 g of 4-[4-(2-tert-butyl-6-cyclobutyl-pyrimidin-4-yl)-piperazin-1-yl]-butylamine (3.18 mmol), and 0.6 g of N-ethyl-N′-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDCl, 3.13 mmol) were added at room temperature, and the reaction mixture was stirred for 16 h. The reaction mixture was then partitioned between water and ethyl acetate. The organic phase was dried over magnesium sulfate, filtered, and concentrated to dryness. The crude product was purified by chromatography on silica gel using dichloromethane-methanol (2-10%). The oily residue was re-dissolved in isopropanol, and 1 N hydrochloric acid in diisopropyl ether was added. The mixture was slowly evaporated to yield 1.0 g of the title compound as a yellowish foam.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08202868B2 |
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| 출처 데이터셋 | uspto-grants-2012_06 |
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| ORD ID | ord-9e0c1c1f13a546c3bc9d5facee701f9b |
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| 출처 메모 | uspto-grants-2012_06 |
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