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Tetrahydrofuran → 3-[(5-ethoxycarbonyl-2-thienyl)-methylene]-2,4(3H,5H)-furandione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Tetronic acid | HCID 521261 | — |
| 反応物 | 4-Ethyl-5-formyl-thiophene-2-carboxylic acid | HCID 20067733 | — |
| 生成物 | 3-[(5-ethoxycarbonyl-2-thienyl)-methylene]-2,4(3H,5H)-furandione | HCID 53806641 | 63% |
反応手順
0.494 gm of tetronic acid (FW=100, 4.94 mmole) and 2.00 gm of ethyl-5-carboxy-2-thiophenecarboxaldehyde (FW=184, 10.9 mole) in 2mL of THF and 10 mL of concentrated HC1 was reacted as before by applying heat and efficient stirring. The total reaction time was 10 minutes. Workup and recrystallization from methanol gave 0.827 gm (63%) of the product. M. p. 204°-205.5° C. C12H10O4S: %C 564.13; %H 3.79; found %C 53.93; %H 4.00. NMR results: 1HNMR (d6DMSO (H2)/TMS δ1.39 (3H, t, 7HZ); 4.39 (2H, q, 7Hz); 7.83 (1H, d, 4Hz); 8.21 (2H, m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04996227 |
| 出典データセット | uspto-grants-1991_02 |
| ORD ID | ord-90d536ed0ea7481fb3e808f3653f70c9 |
| 出典メモ | uspto-grants-1991_02 |