化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → diethyl 3-(m-chlorophenyl)-4-methyl-2-oxo-2H-pyrano[2,3-b]pyridine-6,7-dicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | 3-Chlorophenylacetic acid | HCID 15879 | — |
| 反応物 | Diethyl 5-acetyl-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate | HCID 13752508 | — |
| 溶媒 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | diethyl 3-(m-chlorophenyl)-4-methyl-2-oxo-2H-pyrano[2,3-b]pyridine-6,7-dicarboxylate | HCID 19958197 | 95.1% |
反応手順
Diethyl 5-acetyl-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate (12.0 g, 0.043 mol), 3-chlorophenyl acetic acid (7.33 g, 0.043 mol) and triethylamine (6.52 g) are refluxed in 120 mL of acetic anhydride for three hours. The reaction mixture is cooled, poured into 120 mL of ice-cold water and made alkaline to pH 8 with an ammonium hydroxide solution. The crystalline solid is filtered and washed with water to give (17.0 g, 95%) of the product after drying. Recrystallization from ethyl acetate affords the pure product (13.29, 74% yield), melting point 170°-172° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05622913 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-300e0b1a711340a3858babc405d9b684 |
| 出典メモ | uspto-grants-1997_04 |