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Dimethylformamide → Methyl (3-benzyloxy-5-trifluoromethylthien-2-yl)-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methyl 3-hydroxy-5-(trifluoromethyl)thiophene-2-carboxylate | HCID 2759855 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Methyl (3-benzyloxy-5-trifluoromethylthien-2-yl)-carboxylate | HCID 11278508 | 64% |
反応手順
A mixture of 1B (5.0 g) and dimethylformamide (50 ml) is treated with sodium hydride (1.06 g). Benzylbromide (3.15 ml) was slowly added to the resulting reaction mixture and stirred at room temperature for 20 hours. The reaction mixture was poured into water. The mixture was extracted with diethyl ether twice. The combined organic phases were washed with water, dried and concentrated in vacuo. The crude product was chromatographed (hexane/dichloromethane, 1/1) to give the product as a white solid (4.5 g, 64%) with a melting point of 52°-53.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05869426 |
| 出典データセット | uspto-grants-1999_02 |
| ORD ID | ord-ca532c555b4043f0b2c133c4d9e81124 |
| 出典メモ | uspto-grants-1999_02 |