関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Bromoaniline | HCID 7807 | — |
| 反応物 | 1,4-Bis(4-nitrophenyl)butane-1,4-diyl dimethanesulfonate | HCID 59617179 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(4-Bromophenyl)-2,5-bis(4-nitrophenyl)pyrrolidine | HCID 86649107 | 11% |
反応手順
The product from Example 1C (0.7 g, 1.433 mmol) and 4-bromoaniline (2.54 g, 14.33 mmol) were suspended in DMF (6 mL) and stirred at 50° C. overnight. The resulting mixture was partitioned between ethyl acetate (100 mL) and water (50 mL). The organic phase was washed with 1N HCl (2×50 mL) followed by a brine wash then dried over MgSO4 filtered and concentrated. The crude product was purified by chromatography on silica gel using a solvent gradient of 2-50% ethyl acetate in hexane to give the title compound as a mixture of stereoisomers (74.4 mg, 11% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09006387B2 |
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| 出典データセット | uspto-grants-2015_04 |
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| ORD ID | ord-d687a17fb7b74381b290f1543697476c |
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| 出典メモ | uspto-grants-2015_04 |
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