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Hydrochloric Acid → 3-(4-Hydroxyphenyl)hex-4-ynoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 5-(1-(4-Hydroxyphenyl)but-2-yn-1-yl)-2,2-dimethyl-1,3-dioxane-4,6-dione | HCID 59855133 | — |
| 溶媒 | Pyridine water | HCID 66926435 | — |
| 生成物 | 3-(4-Hydroxyphenyl)hex-4-ynoic acid | HCID 59855136 | 96% |
反応手順
A solution of 5-[1-(4-hydroxyphenyl)but-2-ynyl]-2,2-dimethyl-1,3-dioxane-4,6-dione (20 g, 69.44 mmol) in pyridine-water (5:1, 390 mL) is heated at reflux for 16 hours and after cooling is acidified to pH ˜2 with 5 N HCl and extracted with EtOAc (2×300 mL). The combined extracts are washed with saturated brine, dried over MgSO4, filtered, and concentrated to give an off-white solid (13.5 g, 96%). ESI/MS m/z 203 (M−H)−.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08383642B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-45f98b47da3b415db8f3f616c25e4520 |
| 出典メモ | uspto-grants-2013_02 |