関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formamide | HCID 713 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 5-(2-Bromo-acetyl)-thiophene-3-carboxylic acid methyl ester | HCID 53904546 | — |
| 生成物 | 5-Oxazol-4-yl-thiophene-3-carboxylic acid methyl ester | HCID 58110244 | — |
反応手順
5-(2-Bromo-acetyl)-thiophene-3-carboxylic acid methyl ester (0.60 g, 2.28 mmol) was suspended in formamide (10 mL) then sulfuric acid (1 mL) was added and the tube purged with nitrogen then sealed. The mixture was heated at 150° C. by microwave irradiation for 15 minutes. The resultant solution was diluted with HCl (1 N) and water and extracted with ethyl acetate (×3). The organic phase was dried over sodium sulfate and evaporated then purified by chromatography on a silica II cartridge, eluting with 1:1 DCM:cyclohexane to afford 5-oxazol-4-yl-thiophene-3-carboxylic acid methyl ester as a pale yellow solid (0.197 g). LCMS m/z 210.14 [M+H]+ R. T.=3.64 min (Analytical Method 9).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08614209B2 |
|---|
| 出典データセット | uspto-grants-2013_12 |
|---|
| ORD ID | ord-81f9109593554d81b4f5f8e543e1fb83 |
|---|
| 出典メモ | uspto-grants-2013_12 |
|---|