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HRID 17476作成日:2026年10月26日

Dichloromethane → 7-Fluoro-5-methyl-2-[methyl(pyridin-2-yl)amino]-6-phenyl-1,3-benzoxazole-4-carbonitrile

https://huagongshe.com/reaction/17476

反応式

関与物質

役割名称HCID仕込み量
反応物DichloromethaneHCID 6344—
反応物2-Pyridinamine, N-methyl-HCID 20727—
反応物DiisopropylethylamineHCID 81531—
反応物2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrileHCID 51041429—
溶媒Ethyl AcetateHCID 8857—
生成物7-Fluoro-5-methyl-2-[methyl(pyridin-2-yl)amino]-6-phenyl-1,3-benzoxazole-4-carbonitrileHCID 6858519257.7%

反応条件

温度50 °C

反応手順

Diisopropylethylamine (169 μl, 0.944 mmol) and 2-(methylamino)pyridine (102 μl, 0.994 mmol) were added to a dichloromethane (10 ml) solution of 2-chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-cabonitrile (I-130) (190 mg, 0.663 mmol), followed by heating under reflux in an oil bath at 50° C. for 3 hours. The reaction liquid was cooled to room, temperature, ethyl acetate (70 ml) was added, followed by washing with water (50 ml) and saturated brine (50 ml). After drying over anhydrous sodium sulfate and concentration under reduced pressure, the resulting residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=4:1) to obtain the entitled compound (137 mg, 57.5%) as a colorless solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07737166B2
出典データセットuspto-grants-2010_06
ORD IDord-f1b148179b7e4b379a627f9581f4c5fc
出典メモuspto-grants-2010_06