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6-Methyl-2-pyridylmethanol → (6-methylpyridin-2-yl)methoxycarbonyl-Valine methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 6-Methyl-2-pyridylmethanol | HCID 70736 | — |
| 反応物 | Valine methyl ester | HCID 94285 | — |
| 反応物 | Isocyanate | HCID 105034 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (6-methylpyridin-2-yl)methoxycarbonyl-Valine methyl ester | HCID 70051254 | — |
反応手順
To a solution of the isocyanate derived from Valine methyl ester (17.9 mmol) dissolved in toluene was added 6-methyl-pyridine-2-methanol (2.42 g, 1.1 equivalent). The solution was heated at reflux for 2 hours. After concentration in vacuo and purification by silica gel column chromatography, (6-methylpyridin-2-yl)methoxycarbonyl-Valine methyl ester (2.8 g) was obtained. Hydrolysis of the methyl ester using aqueous lithium hydroxide provide the title compound upon recrystallization from hot ethyl acetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05648497 |
| 出典データセット | uspto-grants-1997_07 |
| ORD ID | ord-9f1622f7f3e84a6e99212258a19a1082 |
| 出典メモ | uspto-grants-1997_07 |