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HRID 17039作成日:2026年10月23日

Potassium Carbonate → [3,5-Bis(trifluoromethyl)benzyl](2-bromo-5-nitrobenzyl)amine

https://huagongshe.com/ja/reaction/17039

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium CarbonateHCID 11430—
反応物3,5-Bis(trifluoromethyl)benzylamineHCID 521099—
反応物Ethyl acetate hexaneHCID 21226206—
反応物2-Bromo-5-nitrobenzyl methanesulfonateHCID 86615392—
溶媒WaterHCID 962—
溶媒DimethylformamideHCID 6228—
生成物[3,5-Bis(trifluoromethyl)benzyl](2-bromo-5-nitrobenzyl)amineHCID 86615393—

反応条件

温度0 °C

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US07737295B2
出典データセットuspto-grants-2010_06
ORD IDord-01c64f527dae46e1bfa7b838e4d4470f
出典メモuspto-grants-2010_06