関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Pyridinecarbonitrile, 1,2-dihydro-4-methoxy-2-oxo- | HCID 2786702 | — |
| 反応物 | 2-Cyclopropylethyl methanesulfonate | HCID 14557809 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-(2-Cyclopropyl-ethyl)-4-methoxy-2-oxo-1,2-dihydro-pyridine-3-carbonitrile | HCID 59272909 | 46% |
反応手順
To a solution of 4-methoxy-2-oxo-1,2-dihydro-pyridine-3-carbonitrile (19.81 g, 131.98 mmol) in acetonitrile (520 ml) were added intermediate 1 (34.36 g, 171.57 mmol) and potassium carbonate (56.73 g, 410.3 mmol) and the mixture was heated at 105° C. for 12 hours. The mixture was cooled to room temperature and the solid was filtered off The filtrate was evaporated till dryness. The crude product was purified by column chromatography (silica gel; DCM to DCM/EtOAc up to 20% as eluent). The desired fractions were collected and evaporated in vacuo to yield intermediate 3 (13.18 g, 46%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08906939B2 |
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| 出典データセット | uspto-grants-2014_12 |
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| ORD ID | ord-19baa36cf228409a8f37bc71082ba742 |
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| 出典メモ | uspto-grants-2014_12 |
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