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Morpholine → Ethyl 2,6-dimethyl-3-(propan-2-yl)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | 3-Methylbutanal | HCID 11552 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | ethyl 4,6-dimethyl-2-oxo-2H-pyran-5-carboxylate | HCID 76918 | — |
| 触媒 | p-Toluenesulfonic acid | HCID 6101 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Ethyl 2,6-dimethyl-3-(propan-2-yl)benzoate | HCID 13126300 | 8.3% |
反応手順
Morpholine (13.34 g), isovaleraldehyde (13.18 g), p-toluene sulfonic acid (0.2 g), and toluene (300 ml) were combined and heated at reflux using a Soxhlet extractor containing magnesium sulfate to remove any water produced. After three hours the Soxhlet extractor was replaced with a condenser, and ethyl 4,6-dimethyl-2-oxo-2H-pyran-5-carboxylate (30 g) was added. The reaction mixture was heated under reflux for approximately 64 hours. The solvent was evaporated, and the resultant oil was distilled at atmospheric pressure to give 11.1 g of crude product which was chromatographed to yield ethyl 2,6-dimethyl-3-(1-methylethyl)benzoate (2.8 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04486588 |
| 出典データセット | uspto-grants-1984_12 |
| ORD ID | ord-22f9ba656ea947e6983cb4244d259aeb |
| 出典メモ | uspto-grants-1984_12 |