関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3,5-Bis(trifluoromethyl)benzylamine | HCID 521099 | — |
| 反応物 | Ethyl acetate hexane | HCID 21226206 | — |
| 反応物 | 2-Bromo-5-nitrobenzyl methanesulfonate | HCID 86615392 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | [3,5-Bis(trifluoromethyl)benzyl](2-bromo-5-nitrobenzyl)amine | HCID 86615393 | — |
反応手順
To a solution of 2-bromo-5-nitrobenzyl methanesulfonate from Step B (0.42 g, 1.35 mmol) and 3,5-bis-trifluoromethyl benzylamine (0.33 g, 1.35 mmol) in DMF (10 ml) at 0° C., potassium carbonate (0.37 g, 2.69 mmol) was added. The mixture was stirred at 0° C. for 2 h. TLC analysis (EtOAc/hexane=2:8) showed completion of the reaction. Water (50 ml) was added. The mixture was extracted with EtOAc (3×40 ml). The combined organic layers were washed with brine, and dried over sodium sulfate. The title compound was obtained by flash column chromatography using 2:8 EtOAc/hexane as the eluant. 1H NMR (CDCl3, 500 MHz) δ 8.35 (d, J=2.5 Hz, 1H), 8.03 (dd, J=8.5, 2.5 Hz, 1H), 7.88 (s, 2H), 7.81 (s, 1H), 8.76 (d, J=8.5 Hz, 1H), 4.00 (s, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07737295B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-01c64f527dae46e1bfa7b838e4d4470f |
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| 出典メモ | uspto-grants-2010_06 |
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