참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-(Hydroxymethyl)-1H-benzimidazole | HCID 78569 | — |
| 반응물 | Bromomethylcyclopropane | HCID 81503 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 69295003 | HCID 69295003 | 26% |
반응 단계
To a solution of (bromomethyl)cyclopropane (0.39 mL, 4.02 mmol) and (1H-benzoimidazol-2-yl)-methanol (596 mg, 4.02 mmol) in DMF (10 mL) was added N,N-diisopropylethylamine (0.84 mL, 4.82 mmol). The reaction mixture was stirred at 60° C. for 3 days. Then it was cooled to room temperature and quenched with saturated NaHCO3 (15 mL) and the phases were separated. The aqueous phase was washed with CH2Cl2 (3×20 mL). Then the combined organic layers were washed with brine (2×30 mL), dried (MgSO4), filtered, concentrated, and dried in vacuo to afford a dark brown oil. Purification by flash column chromatography on silica gel using 2% CH3OH/CH2Cl2 afforded the product as a yellow solid (210 mg, 26%). 1H NMR (CDCl3) δ 0.40-0.45 (m, 2H), 0.52-0.61 (m, 2H), 1.22-1.33 (m, 1H), 4.13 (d, 2H, J=6.6 Hz), 4.88 (s, 2H), 7.22-7.24 (m, 2H), 7.36-7.38 (m, 1H), 7.66-7.69 (m, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07354932B2 |
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| 출처 데이터셋 | uspto-grants-2008_04 |
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| ORD ID | ord-233b25b5575e4ac694bb3ab0eed68b41 |
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| 출처 메모 | uspto-grants-2008_04 |
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