関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | 2,6-Dichloroisonicotinonitrile | HCID 735906 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-Chloro-6-(pyrrolidin-1-yl)pyridine-4-carbonitrile | HCID 83074580 | 87% |
反応手順
A solution of 2,6-dichloropyridine-4-carbonitrile 24 (4 g, 23.5 mmol) in abs. EtOH (10 mL) was added with pyrrolidine (1.15 mL, 1 mol eq) and the mixture was heated at 70° C. for 6 h. The solvent was removed under reduced pressure, water was added to the residue and the aqueous phase was extracted with EtOAc (3×40 mL). The combined organic phase was washed with brine (1×60 mL), dried over Na2SO4 and evaporated to afford 25A as a pale yellow deliquescent solid (4.2 g, 20 mmol, 87% Yield). 1HNMR (DMSO, 400 MHz) δ 2.00 (m, 4H), 3.42 (m, 4H), 6.39 (s, 1H), 6.61 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09409864B2 |
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| 出典データセット | uspto-grants-2016_08 |
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| ORD ID | ord-edd19a8305294f959400d1e5b982b104 |
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| 出典メモ | uspto-grants-2016_08 |
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