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2-Pyridinemethanamine → 4-Hydroxy-6-methyl-1-pyridin-2-ylmethyl-1H-pyridin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Pyridinemethanamine | HCID 19509 | — |
| 反応物 | 4-Hydroxy-6-methyl-2-pyrone | HCID 54675757 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Hydroxy-6-methyl-1-pyridin-2-ylmethyl-1H-pyridin-2-one | HCID 54703055 | 92% |
反応手順
To a suspension of 12.6 g (0.1 mol) of 4-hydroxy-6-methyl-2-pyrone in 50 ml water was added 2-(aminomethyl)pyridine (10.3 ml, 0.1 mol) and the mixture heated to reflux for 2.5 hours. The resulting light yellow compound was filtered from the cooled mixture. Concentration of the filtrate and trituration of the resulting gum with dichloromethane afforded a second crop of the title compound (19.85 g, 92%). NMR (DMSO-d6, ppm): 10.5 (s, 1H), 8.5 (d, 1H), 7.7-7.8 (t, 1H), 7.2 (t, 1H), 7.1 (d, 1H), 5.8 (s, 1H), 5.5 (s, 1H), 5.2 (s, 2H), 2.2 (s, 3H). FIA: m/z-215.1 ES−/217.1 ES+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07727992B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-81533076c8b148cfa53adb9113171694 |
| 出典メモ | uspto-grants-2010_06 |