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Dimethylformamide → Methyl 4-(5-(4-(pentyloxy)phenyl)isoxazol-3-yl)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | 1-Amino-1-(4-methoxycarbonylphenyl)-3-oxo-3-(4-pentyloxyphenyl)-1-propene | HCID 69677713 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Methyl 4-(5-(4-(pentyloxy)phenyl)isoxazol-3-yl)benzoate | HCID 10737571 | 95.2% |
反応手順
Dimethylformamide (44 ml), 1-amino-1-(4-methoxycarbonylphenyl)-3-oxo-3-(4-pentyloxyphenyl)-1-propene (5.5 g) and hydroxylamine hydrochloride (2.0 g) were charged in 300-ml three-necked flask at room temperature and heated, and the reaction was carried out at the inner temperature of 55 to 60° C. for 4 hours. After completion of the reaction, the mixture was cooled down to room temperature, and acetonitrile (110 ml) was added to separate the crystals. The inner temperature was made 0 to 5° C., and the crystals were filtered and washed with acetonitrile (28 ml) and water (110 ml). The crystals were dried overnight in vacuo to give methyl 4-[5-(4-pentyloxyphenyl)isoxazol-3-yl]benzoate (5.21 g)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06455726B2 |
| 出典データセット | uspto-grants-2002_09 |
| ORD ID | ord-1137a9ad34b14f2e9ba0c5523e8d7118 |
| 出典メモ | uspto-grants-2002_09 |