化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 4-(2-Hydroxy-2-methylpropyl)phenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 4-Hydroxyphenylacetone | HCID 7019274 | — |
| 反応物 | HCID 178418573 | HCID 178418573 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-(2-Hydroxy-2-methylpropyl)phenol | HCID 13481807 | 77% |
反応手順
To a solution of methyl magnesium bromide (3 M, 14 mL, 39.94 mmol) cooled to 0° C. was added tetrahydrofuran (10 mL) and as solution of 1-(4-hydroxy-phenyl)-propan-2-one (1 g, 6.66 mmol) in tetrahydrofuran (30 mL). The resulting mixture was then warmed to room temperature and then stirred for 2 h. At this time, the reaction was partioned between ethyl acetate and water. The water layer was made acidic with 1N aqueous hydrochloric acid (pH=1). The organic phase was separated and concentrated in vacuo. The residue was dissolved in a small volume of tetrahydrofuran and the mixture was treated with an excess of hexanes. This resulted in the precipitation of the product 4-(2-hydroxy-2-methyl-propyl)-phenol (0.85 g, 77%) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741327B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-ec8ba2c472af48de883088e447b5e0af |
| 出典メモ | uspto-grants-2010_06 |