참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 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,N-dimethylacetamide | HCID 68193281 | 76.5% |
반응 단계
(4′-Bromobiphenyl-4-yl)acetic acid (1.0 g, 3.4 mmol) was dissolved in a mixed solvent of tetrahydrofuran (20 mL) and methanol (20 mL), and dimethylamine hydrochloride (0.42 g, 5.2 mmol), 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride (1.3 g, 4.7 mmol) and N-methylmorpholine (0.95 mL, 8.6 mmol) were added, followed by stirring at room temperature for 18 hours. After the reaction solution was concentrated under reduced pressure, the resulting residue was purified by chromatography on a silica gel column (Moritex Corporation, elution solvent: dichloromethane/ethyl acetate), and a fraction corresponding to the Rf value=0.55 (dichloromethane/ethyl acetate=1/1) by thin layer chromatography was concentrated under reduced pressure to afford the title compound (0.82 g, 2.6 mmol) as a white solid (yield 75%).
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-592cbb6cc2b04eb198e76dc0694769d9 |
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| 출처 메모 | uspto-grants-2014_07 |
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