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Water → 5-(3-Oxo-1-phenylbutyl)-4-phenyl-2-oxo-4-oxazoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | 4-Phenyl-3-Buten-2-one | HCID 15909 | — |
| 反応物 | 4-Oxazolin-2-one, 4-phenyl- | HCID 118669 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 5-(3-Oxo-1-phenylbutyl)-4-phenyl-2-oxo-4-oxazoline | HCID 15541756 | 86.3% |
反応手順
To a solution of 4-phenyl-2-oxo-4-oxazoline (1.61 g) and benzalacetone (1.46 g) in acetonitrile (20 ml) was added dropwise methanesulfonic acid (0.96 g). After stirring the obtained mixture at room temperature for 30 min, water was added, and the mixture was extracted with ethyl acetate. The extract was washed with water and dried (MgSO4), and the solvent was evaporated. The residue was subjected to silica gel column chromatography and eluted with hexane-ethyl acetate (1:1). The solvent was evaporated. Crystallization from isopropyl ether gave 4-(4-phenyl-2-oxo-4-oxazolin-5-yl)-4-phenyl-2-butanone (2.65 g; yield 86.3%). Recrystallization from ethanol gave colorless crystals.
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-547f94840dbf42e1b5c1663b995de3f7 |
| 出典メモ | uspto-grants-2004_03 |