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N-bromobutanimide → Ethyl 5-bromo-4-(p-chlorophenyl)pyrrole-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | ethyl 4-(4-chlorophenyl)-1H-pyrrole-3-carboxylate | HCID 470434 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 5-bromo-4-(p-chlorophenyl)pyrrole-3-carboxylate | HCID 15010185 | 90,348.398% |
反応手順
Ethyl 4-(p-chlorophenyl)pyrrole-3-carboxylate (1.6 g., 0.0064 mmol) is dissolved in tetrahydrofuran (40 mL). N-bromosuccinimide (1.14 g., 0.0064 mmol) is added in small portions at 25°-28° C. After the addition is complete, the solution is stirred overnight at room temperature. The solution is concentrated in vacuo and the solid residue partioned between water and ether. The ether layer is separated and dried over magnesium sulfate. Work-up of the ether extract leaves 1.9 g (90%) of a white solid which is purified by stirring with a mixture of 80/20 hexane/ethyl acetate. The insoluble solid (1.3 g, 62%) is collected and has m.p. 161°-164° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05310938 |
| 出典データセット | uspto-grants-1994_05 |
| ORD ID | ord-ad8d558a86874856becc73421c1a1ec8 |
| 出典メモ | uspto-grants-1994_05 |