化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Carbonate → Methyl 3-(4-ethoxycarbonylmethylsulfanylphenoxymethyl)thiophene-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl 2-[(4-hydroxyphenyl)sulfanyl]acetate | HCID 3742252 | — |
| 反応物 | Methyl 3-(bromomethyl)thiophene-2-carboxylate | HCID 10537693 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 3-(4-ethoxycarbonylmethylsulfanylphenoxymethyl)thiophene-2-carboxylate | HCID 68571726 | 80% |
反応手順
Methyl 3-bromomethylthiophene-2-carboxylate (28.2 ml, 120 mmol) and potassium carbonate (36.6 g, 264 mmol) were added to a DMF (300 mL) solution of the compound obtained in Example 18 (28.1 g, 132 mmol), and the mixture was stirred overnight at room temperature. The solvents were distilled off under a reduced pressure, water was added to the residue, and the product was extracted with ethyl acetate. The organic layer was washed with a saturated sodium chloride solution, and then dried over anhydrous sodium sulfate, and the solvents were distilled off under a reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1), to give 35.1 g (80%) of the captioned compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08377967B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-c785325008a24a1a9f199a75b8555173 |
| 出典メモ | uspto-grants-2013_02 |