참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 반응물 | 4'-Bromo-4-carboxymethylbiphenyl | HCID 1394245 | — |
| 반응물 | 4-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride | HCID 2734059 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-(4'-Bromobiphenyl-4-yl)-N-methoxy-N-methylacetamide | HCID 86670083 | 100% |
반응 단계
(4′-Bromobiphenyl-4-yl)acetic acid (12 g, 37 mmol) was dissolved in a mixed solvent of tetrahydrofuran (200 mL) and methanol (200 mL), and N,O-dimethylhydroxylamine hydrochloride (5.4 g, 56 mmol), 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride (15 g, 60 mmol) and N-methylmorpholine (6.1 mL, 56 mmol) were added, followed by stirring at room temperature for 1 hour. After the reaction solution was concentrated under reduced pressure, ethyl acetate was added to the resulting residue, and the organic layer was washed with water. After the solvent was distilled off under reduced pressure, the resulting residue was purified by chromatography on a silica gel column (Moritex Corporation, elution solvent: hexane/ethyl acetate), and a fraction corresponding to the Rf value=0.45 (hexane/ethyl acetate=1/1) by thin layer chromatography was concentrated under reduced pressure to afford the title compound (12 g, 37 mmol) as a white solid (yield 100%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08785462B2 |
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| 출처 데이터셋 | uspto-grants-2014_07 |
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| ORD ID | ord-2d614cf624984dca89529b848563f4ae |
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| 출처 메모 | uspto-grants-2014_07 |
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