関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Chlorobenzyl mercaptan | HCID 80409 | — |
| 反応物 | 4-Chloropyridin-2-ol | HCID 2757611 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(4-chlorobenzylthio)pyridin-2(1H)-one | HCID 58580248 | — |
反応手順
A mixture of 4-chloropyridin-2(1H)-one (100 mg, 0.77 mmol), K2CO3 (320 mg, 2.32 mmol) and (4-chlorophenyl)methanethiol (612 mg, 3.86 mmol) was stirred at 100° C. for 18 hours. After cooling the reaction to RT and was dilution with CH2Cl2 (5 mL), the crude product was subjected to flash chromatography (silica gel/hexane-EtOAc 100:0 to 0:100 gradient, employing LC-MS to identify the fractions containing the desired product) to afford 4-(4-chlorobenzylthio)pyridin-2(1H)-one 8A (96 mg, 46.9% yield). 1H NMR (400 MHz, Chloroform-D) δ ppm 12.30 (1H, br. s.), 7.28-7.43 (4H, m), 7.15 (1H, d, J=7.03 Hz), 6.28 (1H, d, J=1.51 Hz), 6.11 (1H, dd, J=6.90, 1.88 Hz), 4.11 (2H, s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08563583B2 |
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| 出典データセット | uspto-grants-2013_10 |
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| ORD ID | ord-eaece1f5915746189f97693d48383c3f |
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| 出典メモ | uspto-grants-2013_10 |
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