化工社化工社 化学情報印刷レポート · 研究参考用
Isobutyrophenone → 1-(2-Methoxy-3,4,6-trimethylphenyl)-1-phenyl-2-methylpropanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isobutyrophenone | HCID 69144 | — |
| 反応物 | 2-Bromo-3,5,6-trimethylanisole | HCID 21961310 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(2-Methoxy-3,4,6-trimethylphenyl)-1-phenyl-2-methylpropanol | HCID 10542111 | 80.2% |
反応手順
A solution of 2-bromo-3,5,6-trimethylanisole (3.0 g, 13.1 mmol) in tetrahydrofuran (20 ml) was cooled to -78° C. and n-butyllithium (1.6M solution in hexane, 8.2 ml, 13.1 mmol) was added dropwise. The reaction mixture was stirred at the same temperature for 15 minutes. Then a solution of isobutyrylbenzene (1.94 g, 13.1 mmol) in tetrahydrofuran (5 ml) was added dropwise and the resulting mixture was stirred at room temperature for additional 30 minutes. The reaction mixture was diluted with water and the product was extracted with isopropyl ether. The extract was washed with water, dried and then concentrated. The residue was crystallized from hexane to obtain the desired compound (3.13 9, yield: 80.2%), m.p. 80°-81° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05770772 |
| 出典データセット | uspto-grants-1998_06 |
| ORD ID | ord-6bb4885f6e5f42fda767c881791cc75f |
| 出典メモ | uspto-grants-1998_06 |