関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenyl isocyanate | HCID 7672 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Allylmorpholine | HCID 136522 | — |
| 反応物 | 2-(2-Nitroethoxy)tetrahydropyran | HCID 3748656 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | [5-((Morpholin-4-yl)methyl)-4,5-dihydro-isoxazol-3-yl]methyl 2-tetrahydropyranyl ether | HCID 21978771 | 44.3% |
反応手順
To a solution of N-allylmorpholine (0.76 g, 5.0 mmol) in toluene (10 mL) was added 2-(2-nitroethoxy)tetrahydropyran (1.34 g, 7.7 mmol), phenylisocyanate (2:43 g, 20.1 mmol), and triethylamine (52 mg; 0.5 mmol). The resulting mixture was heated at 55° C. overnight. After cooling to room temperature the formed precipitate was removed by filtration and the remaining solution concentrated in vacuo. The residue was purified by flash chromatography (SiO2, CH2Cl2/MeOH/NH4OH 96/3.75/0.25) to yield 0.63 g (44%) of [5-((morpholin-4-yl)methyl)-4,5-dihydro-isoxazol-3-yl]methyl 2-tetrahydropyranyl ether. MH+ 285, Rf 0.34 (CH2Cl2/MeOH/NH4OH 96/3.75/0.25).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07094779B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-f898d1d16b634156866bfd923aef5933 |
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| 出典メモ | uspto-grants-2006_08 |
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