関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methyl 4-nitrobutyrate | HCID 25604 | — |
| 反応物 | 1,4-Diisocyanatobenzene | HCID 61009 | — |
| 反応物 | Benzene, 1-methoxy-4-(3,3,3-trifluoro-1-propynyl)- | HCID 11333117 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-(Trifluoromethyl)isoxazole | HCID 13739401 | 56.5% |
反応手順
1,4-Phenylene diisocyanate (597.1 mg, 3.73 mol) and triethylamine (780 μL, 5.60 mmol) were added to a solution of 1-methoxy-4-trifluoropropynylbenzene (373.2 mg, 1.86 mmol) and 4-nitrobutanoic acid methyl ester (441.5 mg, 2.80 mmol) in toluene (10 mL). Using a microwave reactor, the obtained mixture was stirred at 150° C. for 2 hours. The reaction solution was filtered with celite, and the solvent was then distilled away. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to obtain a trifluoromethyl isoxazole compound (144.0 mg, yield: 25%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08648103B2 |
|---|
| 出典データセット | uspto-grants-2014_02 |
|---|
| ORD ID | ord-2e26deebd655408b90e6dec23afdcba7 |
|---|
| 出典メモ | uspto-grants-2014_02 |
|---|
