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HRID 594070作成日:2026年10月26日

1,2-Dichloroethane → 3-bromo-4-(hydroxymethyl)-N-(3-(trifluoromethyl)phenyl)benzamide

https://huagongshe.com/reaction/594070

反応式

関与物質

役割名称HCID仕込み量
反応物1,2-DichloroethaneHCID 11—
反応物3-(Trifluoromethyl)anilineHCID 7375—
反応物HOAtHCID 181649—
反応物3-Bromo-4-(hydroxymethyl)benzoic acidHCID 19688415—
溶媒WaterHCID 962—
溶媒DimethylformamideHCID 6228—
生成物3-bromo-4-(hydroxymethyl)-N-(3-(trifluoromethyl)phenyl)benzamideHCID 9040796335%

反応手順

EDC (1.3 equiv.) was added to a solution of 3-bromo-4-(hydroxymethyl)benzoic acid (1.0 equiv), 3-(trifluoromethyl)aniline (1.1 equiv.), HOAt (1.3 equiv.) in DMF (0.43 M). The mixture was stirred at ambient temperature 3 hrs. The reaction mixture was diluted with water and extracted with ethyl acetate. The combined extracts were washed sequentially with 1M aqueous sodium hydroxide and brine, dried over sodium sulfate, filtered, and concentrated. The residue was purified by ISCO(50% EtOAc/Heptane) to yield 3-bromo-4-(hydroxymethyl)-N-(3-(trifluoromethyl)phenyl)benzamide in 35% yield. LC/MS (m/z)=374.0 (MH+), Rt=0.93 min.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09242969B2
出典データセットuspto-grants-2016_01
ORD IDord-97272b5ef77b4a53bcffe989e86abaa7
出典メモuspto-grants-2016_01