化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 4-Methyl-5-phenyl-2-p-tolyloxazole 3-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Methylbenzaldehyde | HCID 7725 | — |
| 反応物 | 1,2-Propanedione, 1-phenyl-, 2-oxime | HCID 6399024 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 4-Methyl-5-phenyl-2-p-tolyloxazole 3-oxide | HCID 58934191 | — |
反応手順
12.5 g of 1-phenyl-1,2-propanedione-2-oxime and 10 ml of p-tolualdehyde are added to 50 ml of glacial acetic acid, and HCl gas is introduced for 30 minutes, with ice-cooling. The product is precipitated as the hydrochloride by addition of methyl tert-butyl ether and filtered off with suction, and the precipitate is washed with methyl tert-butyl ether. The precipitate is suspended in water and the pH is made alkaline using ammonia. The mixture is extracted three times with in each case 200 ml of dichloromethane, the combined organic phases are dried over MgSO4 and the solvent is then removed under reduced pressure. This gives 6.4 g of 4-methyl-5-phenyl-2-p-tolyloxazole 3-oxide as a white solid. C17H15NO2 (265.31), MS(ESI)=266 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07365084B2 |
| 出典データセット | uspto-grants-2008_04 |
| ORD ID | ord-c6d8bd31b53646a082a941b63e8f693b |
| 出典メモ | uspto-grants-2008_04 |