関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl 2,6-dimethylnicotinate | HCID 351337 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (2,6-Dimethylpyridin-3-yl)methanol | HCID 2784752 | — |
反応手順
To a solution of ethyl 2,6-dimethylnicotinate (1.0 g, 5.6 mmol) in THF (20 mL) at 0° C. was added LiAlH4 (318 mg, 8.4 mmol). The resulting mixture was stirred at 0° C. for 5 min and then warmed to room temperature for 1 hour. Quenched with 0.3 mL water, 0.3 mL 15% NaOH solution and then with 1 mL water sequentially. After stirred at room temperature for 15 min, sodium sulfate was added to the mixture and stirred for another 15 min and then filtered. The resulting solution was concentrated to afford the crude product which was used for next step directly without further purification. LCMS (ESI) m/z=138.1 138.1 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09353104B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-320884b0c7b94f92985f0c5481abe8f9 |
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| 出典メモ | uspto-grants-2016_05 |
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