関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | Ethyl 6-difluoromethoxymethylpyridine-2-carboxylate | HCID 66718372 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-Pyridinemethanol, 6-[(difluoromethoxy)methyl]- | HCID 66718418 | 80% |
反応手順
NaBH4 (377 mg, 9.96 mmol) was added to a solution of ethyl 6-difluoromethoxymethylpyridine-2-carboxylate (2.30 g, 9.96 mmol) in EtOH (50 mL) at 0° C., the mixture was warmed to 80° C. and stirred for 5 h. The mixture was cooled to 0° C., quenched with sat. aq. NH4Cl, concentrated in vacuo and partitioned between EtOAc and brine. The organic layer was separated, dried (MgSO4), filtered and evaporated to give the title compound (1.50 g, 80%) as a colorless oil; NMR δH (400 MHz, CDCl3) 7.73 (1H, t, J 8.0 Hz), 7.35 (1H, d, J 8.0 Hz), 7.19 (1H, d, J 8.0 Hz), 6.39 (1H, t, J 74.0 Hz), 5.02 (2H, s), 4.76 (2H, s); (M+H)+ 190.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08987279B2 |
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| 出典データセット | uspto-grants-2015_03 |
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| ORD ID | ord-6cd9753ac33f4a8a962a097181733aaf |
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| 出典メモ | uspto-grants-2015_03 |
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