関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 2-Thiopheneacetyl chloride | HCID 162362 | — |
| 反応物 | Mls002704122 | HCID 268729 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1,3-Dibenzyl-5-(2-thienylacetyl)barbituric acid | HCID 9889035 | 70.8% |
反応手順
To a solution of 1,3-dibenzylbarbituric acid 154 mg (0.500 mmol) in dry dichloromethane 2.0 mL under a nitrogen atmosphere, added was pyridine 1.0 mL (12 mmol) and stirred at 0° C. Added was 2-thienylacetyl chloride 80 mg (0.50 mmol, 1.00 equivalent) in dichloromethane 1.0 mL to the solution slowly during a period of 20 minutes, then stirred at room temperature for 3 hours. Added was ether 50 mL and washed the organic layer with 2 M hydrochloric acid and saturated brine, and dried over sodium sulfate. Purified was the crude product 216 mg after removal of the solvent under the reduced pressure, by column chromatography (silica gel, eluted with dichloromethane). It obtained 1,3-dibenzyl-5-(2-thienylacetyl)barbituric acid 153 mg as yellow viscous oil (56.9% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06498164B1 |
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| 出典データセット | uspto-grants-2002_12 |
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| ORD ID | ord-3c1f3b0149b84b2bb77617a4f1ff0a3c |
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| 出典メモ | uspto-grants-2002_12 |
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