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2-Butenoic acid, 3-amino-, ethyl ester, (2Z)- → 1,4-Dihydro-2,6-dimethyl-4-(2-methylbenzo[b]thien-3-yl)-3,5-pyridinedicarboxylic acid, diethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Butenoic acid, 3-amino-, ethyl ester, (2Z)- | HCID 643756 | — |
| 反応物 | 2-Methyl-1-benzothiophene-3-carbaldehyde | HCID 3775467 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1,4-Dihydro-2,6-dimethyl-4-(2-methylbenzo[b]thien-3-yl)-3,5-pyridinedicarboxylic acid, diethyl ester | HCID 13826854 | 43.1% |
反応手順
A mixture of 2.2 g of 2-methylbenzo[b]thiophene-3-carboxaldehyde, 4.9 g of ethyl 3-aminocrotonate, and 10 ml of ethanol were heated to reflux for approximately 18 hours. An additional 1.6 g of ethyl 3-aminocrotonate were added and the reaction was heated an additional 24 hours at reflux. The reaction mixture was cooled and concentrated and the resulting solid was recovered by filtration providing 2.15 g of the desired title product, m.p. 191°-193° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04659717 |
| 出典データセット | uspto-grants-1987_04 |
| ORD ID | ord-1d3dcd6e82f24cff84d6d8aa644653d9 |
| 出典メモ | uspto-grants-1987_04 |