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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-toluenesulfonic acid (0.2 g), and toluene (300 ml) were combined and heated at reflux using a Soxhlet extractor with 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 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 | US04375476 |
| 出典データセット | uspto-grants-1983_03 |
| ORD ID | ord-3deaa738e08b489ea56184426ebd4810 |
| 出典メモ | uspto-grants-1983_03 |