関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Oxan-2-amine | HCID 14471248 | — |
| 反応物 | 2-(4-Fluoro-3-nitrophenyl)benzoxazole | HCID 21990970 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-(Benzoxazol-2-yl)-2-(tetrahydropyran-4-yl)nitrobenzene | HCID 67498108 | 63.7% |
反応手順
5-(Benzoxazol-2-yl)-2-fluoronitrobenzene (see Working Example 15-2) (0.55 g, 2.13 mmol), triethylamine (0.26 g, 2.57 mmol), and aminotetrahydropyran (0.24 g, 2.34 mmol) were added to ethanol (10 mL), and this reaction mixture liquid was heated to reflux with stirring for 2 hours. The reaction mixture was cooled to room temperature and was concentrated under reduced pressure, and 0.1N aqueous hydrochloric acid solution (50 mL) was added to the residue obtained, this was successively extracted with ethyl acetate (approx. 50 mL, 4 times), washed with water (30 mL), and dried over anhydrous sodium sulfate, and the solvent was distilled off at reduced pressure. The residue obtained was purified by silica gel column chromatography to yield the title compound (440 mg, 60.9% yield) as light brown crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08829035B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-6875da00e67c46a6a16d50b8bf7dbae0 |
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| 出典メモ | uspto-grants-2014_09 |
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