化工社化工社 化学情報印刷レポート · 研究参考用
Dimethyl oxalate → Ethyl 4-(6-methyl-3-pyridyl)-2,4-dioxobutanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl oxalate | HCID 11120 | — |
| 反応物 | 3-Acetyl-6-methylpyridine | HCID 95292 | — |
| 反応物 | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| 反応物 | LiHMDS tetrahydrofuran | HCID 23714775 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 4-(6-methyl-3-pyridyl)-2,4-dioxobutanoate | HCID 23143403 | — |
反応手順
At −78° C., a tetrahydrofuran (5 ml) solution of 5-acetyl-2-picoline (583 mg) was added to a tetrahydrofuran (15 ml) solution of 1 N lithium hexamethyldisilazide/tetrahydrofuran solution (5.2 ml), and stirred at the same temperature for 1 hour. At −78° C., dimethyl oxalate (701 μl) was added to the reaction liquid, and stirred at room temperature for 1 hour. 4 N hydrogen chloride/dioxane solution (4 ml) was added to the reaction liquid, and concentrated under reduced pressure to obtain a crude product of the entitled compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07829586B2 |
| 出典データセット | uspto-grants-2010_11 |
| ORD ID | ord-98e579a05ecf4d00ba816fa58c4b447d |
| 出典メモ | uspto-grants-2010_11 |