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O-Cresol → 2-(2-Methyl-1-imidazolyl)-5-[3-(2-methylphenoxy)propyl]-4-(4-trifluoromethylphenyl)oxazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | O-Cresol | HCID 335 | — |
| 反応物 | Tributylphosphine | HCID 13831 | — |
| 反応物 | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| 反応物 | 2-(2-Methyl-1-imidazolyl)-4-(4-trifluoromethylphenyl)-5-oxazolepropanol | HCID 23431807 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(2-Methyl-1-imidazolyl)-5-[3-(2-methylphenoxy)propyl]-4-(4-trifluoromethylphenyl)oxazole | HCID 23431806 | — |
反応手順
To a mixture of 2-(2-methyl-1-imidazolyl)-4-(4-trifluoromethylphenyl)-5-oxazolepropanol (700 mg), 2-methylphenol (432 mg), tributylphosphine (607 mg) and tetrahydrofuran (10 mL) was added 1,1′-(azodicarbonyl)dipiperidine (750 mg) at room temperature and the mixture was stirred for 1 h. The reaction mixture was concentrated and the residue was subjected to silica gel column chromatography. The title compound was obtained as crystals from an eluate from ethyl acetate-hexane (2:3, v/v). Recrystallization from acetone-isopropyl ether gave colorless prism crystals (591 mg, 67%). melting point: 101-102° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06699995B1 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-bc760dbfe90040c3863612e77cd9249f |
| 出典メモ | uspto-grants-2004_03 |