関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Ethyl 1H-pyrrole-2-carboxylate | HCID 255670 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | Ethyl 4-bromopyrrole-2-carboxylate | HCID 5324607 | — |
反応手順
1H-Pyrrole-2-carboxylic acid ethyl ester (10 g) was dissolved in carbon tetrachloride (50 ml). A carbon tetrachloride solution (50 ml) of bromine was added dropwise thereto on ice over 30 minutes. The reaction mixture was stirred at 25° C. for one hour. The suspension of reaction mixture was added dropwise to an ethanol solution (100 ml) of 10% sodium ethoxide on ice over 20 minutes. The solvent was concentrated under reduced pressure. The resulting residue was diluted with ethyl acetate (40 ml) and water (20 ml). The organic layer was washed with an aqueous solution saturated with sodium chloride (10 ml), and then concentrated. The residue obtained by concentration under reduced pressure was purified by silica gel column chromatography (hexane/ethyl acetate). Thus, a brown solid was obtained (10 g, 99%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08829199B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-fd68bc68f7e64f2d868a563444a0b180 |
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| 出典メモ | uspto-grants-2014_09 |
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