関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,4-Diethoxybenzamide | HCID 340342 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-(Bromoacetyl)pyridine hydrobromide | HCID 2776239 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(3,4-Diethoxyphenyl)-4-(pyridin-4-yl)oxazole | HCID 59145490 | 2.7% |
反応手順
In a microwave vial were dissolved 2-bromo-1-(pyridin-4-yl)ethanone hydrobromide (134 mg, 0.478 mmol) and 3,4-diethoxybenzamide (100 mg, 0.478 mmol) in DMF (5 ml) and the reaction was heated at 170° C. for 40 min. The reaction mixture was poured in a saturated solution of NaHCO3 and extracted with EtOAc (50 ml×3). The combined organic phases were washed with a saturated solution of NaCl (2×30 ml) and concentrated under reduced pressure. The product was purified by column chromatography using CH2Cl2:MeOH (95:5) to yield 4 mg (2.7%) of the product. MS (EI) m/z: 311 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08530503B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-0535fb29f7d64ec2b5bb1177c386bf20 |
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| 出典メモ | uspto-grants-2013_09 |
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