関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dibromoethane | HCID 7839 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 5-(Benzyloxy)-2-(hydroxymethyl)-1,4-dihydropyridin-4-one | HCID 2801564 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (2,3-Dihydro-[1,4]dioxino[2,3-c]pyridin-7-yl)methanol | HCID 21873770 | — |
反応手順
A solution of 5-Benzyloxy-2-hydroxymethyl-1H-pyridin-4-one (2 g, 8.7 mmol) in water (220 mL) containing sodium hydroxide (17 mmol) was hydrogenated over 10% palladium on charcoal (1 g) for 4 hours. The mixture was filtered and evaporated to give a white solid. This solid was dissolved in N,N-dimethylformamide (8 mL) then treated with potassium carbonate (2.9 g) and 1,2-dibromoethane (0.6 mL, 7 mmol). The mixture was heated at 85° C. overnight. The cooled mixture was evaporated onto silica and chromatographed eluting with 10-30% methanol in ethyl acetate affording a white solid (250 mg, 21%); MS (APCl+) m/z 168 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07691850B2 |
|---|
| 出典データセット | uspto-grants-2010_04 |
|---|
| ORD ID | ord-7e03b8c7a8094f4ca56b53ceea538794 |
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| 出典メモ | uspto-grants-2010_04 |
|---|
