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Sodium Carbonate → N-(4-Bromo-2,6-dichloro-phenyl)-2-cyclopentyl-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 4-Bromo-2,6-dichloroaniline | HCID 69680 | — |
| 反応物 | Cyclopentylacetyl chloride | HCID 3485182 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-(4-Bromo-2,6-dichloro-phenyl)-2-cyclopentyl-acetamide | HCID 68711978 | 80% |
反応手順
4-Bromo-2,6-dichloroaniline (12.1 g) and cyclopentylacetyl chloride (8.1 g) were dissolved in tetrahydrofuran (100 mL) and sodiumcarbonate (6.4 g) is added, followed by heating to reflux for 6 hours. The reaction mixture was cooled to ambient temperature and filtered and diluted with water (250 ml). After extraction, the combined organic phase was concentrated in vacuo to furnish 14.0 g (80% yield) of the title compound as a white solid. LC-MS (m/z) 352 (MH+); tR=3.47, (UV, ELSD) 96%, 99%. 1H NMR (500 MHz, DMSO-d6): 1.12 (m, 2H), 1.50 (m, 4H), 1.80 (m, 2H), 2.15 (m, 1H), 2.50 (d, 2H), 5.70 (broad s, 1H), 7.45 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07601870B2 |
| 出典データセット | uspto-grants-2009_10 |
| ORD ID | ord-97f69c1dc8f144b8a7615fd4c1f61766 |
| 出典メモ | uspto-grants-2009_10 |