関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Cyclohexane, (bromomethyl)- | HCID 137636 | — |
| 反応物 | 5-(4-Methoxyphenyl)pyridin-2(1H)-one | HCID 20081497 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-(cyclohexylmethyl)-5-(4-methoxyphenyl)pyridin-2(1H)-one | HCID 58966919 | 31.4% |
反応手順
According to Scheme 5 Step 2: To a solution of 5-(4-methoxyphenyl)pyridin-2(1H)-one (1 eq, 0.35 mmol, 70 mg, Example 7 Step 1) in acetonitrile (2 mL) were added K2CO3 (10 eq, 3.50 mmol, 0.48 g) and (bromomethyl)cyclohexane (10 eq, 3.50 mmol, 0.49 mL). The reaction was microwaved for 10 minutes at 180° C. The reaction was allowed to cool. The reaction was then filtered and concentrated under reduced pressure. The crude product was purified by flash chromatography over silica gel (AIT Flashsmart prepacked column 15 g SiO2) using CH2Cl2/AcOEt (80/20, Rf=0.3). The product was further purified by reverse phase C18 column using water/acetonitrile 60/40 to afford 1-(cyclohexylmethyl)-5-(4-methoxyphenyl)pyridin-2(1H)-one (0.11 mmol, 32 mg, 31%) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08399493B2 |
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| 出典データセット | uspto-grants-2013_03 |
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| ORD ID | ord-f1a033baa6394e649dbefcb8b87bcc82 |
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| 出典メモ | uspto-grants-2013_03 |
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