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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
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 2-Pyridinamine, N-methyl- | HCID 20727 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Chloro-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile | HCID 51041429 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 7-Fluoro-5-methyl-2-[methyl(pyridin-2-yl)amino]-6-phenyl-1,3-benzoxazole-4-carbonitrile | HCID 68585192 | 57.7% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07737166B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-f1b148179b7e4b379a627f9581f4c5fc |
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| 出典メモ | uspto-grants-2010_06 |
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