참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2,6-Dichloropyrazine | HCID 78504 | — |
| 반응물 | (S)-1-(3,4-Difluorophenyl)ethanamine | HCID 7016601 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 6-chloro-N-[(1S)-1-(3,4-difluorophenyl)ethyl]pyrazin-2-amine | HCID 58869933 | 35.1% |
반응 단계
(1S)-1-(3,4-Difluorophenyl)ethanamine (977 mg, 6.2 mmol) and 2,6-dichloropyrazine (1.236 g, 8.3 mmol, 1.3 eq) was dissolved in dioxane (5 mL) and potassium carbonate (1.73 g, 2.0 eq) added to the solution. The mixture was then heated at reflux (110° C.) under a nitrogen atmosphere for 65 hours. The crude reaction mixture was then poured onto cold water (30 mL) and extracted with diethyl ether (3×30 mL). The combined organic extracts were concentrated and subjected to flashmaster chromatography (20 g silica cartridge (8:2 petroleum spirits:ethyl acetate, followed by ethyl acetate flush) to afford the desired pyrazine-adduct as an off-white solid (587 mg, 35%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07737143B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-6509b31877f84ef2b22f7be7512ab378 |
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| 출처 메모 | uspto-grants-2010_06 |
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