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Sulfuric Acid → 7-Hydroxy-4-benzopyrone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3-chloro-1-(2,4-dihydroxyphenyl)propan-1-one | HCID 11805742 | — |
| 生成物 | 7-Hydroxy-4-benzopyrone | HCID 5409279 | 88% |
反応手順
To a cooled (5° C.) solution of 2N sodium hydroxide (10.0 L) was added the compound of step A (244.1 g) in one portion. The solution was warmed to room temperature over 2 hours using a warm water bath then recooled to 5° C. and the pH adjusted to 2 with 6M sulfuric acid (1.2 L). The mixture was extracted with 3×3.0 L of ethyl acetate, washed with brine (1×2.0 L) dried over sodium sulfate and filtered. Concentration in vacuo gave a tan solid. Trituration with hexanes, and filtration afforded 173.7 g (58% yield) of the title compound. M.P. 136° C.-137° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05552435 |
| 出典データセット | uspto-grants-1996_09 |
| ORD ID | ord-850973f56ac44474b4b10b2933702cb0 |
| 出典メモ | uspto-grants-1996_09 |