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Methanol → Benzoic acid, 3,5-dimethyl-, methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 3,5-Dimethylbenzoic acid | HCID 10356 | — |
| 生成物 | Benzoic acid, 3,5-dimethyl-, methyl ester | HCID 32786 | 90% |
反応手順
A solution of 3,5-dimethyl benzoic acid (25 g, 0.17 mol) in methanol (250 ml) was treated with sulfuric acid (1 ml, cat. amount) and heated to reflux. After 10 hours, the solution was cooled to room temperature, concentrated to approximately 1/2 volume and poured into 200 ml of crushed ice. The mixture was extracted twice with 200 ml portions of diethyl ether. The organic phase was extracted with saturated aqueous sodium carbonate, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting solid was recrystallized from hexanes to yield the product (24.5 g, 90% yield) as volatile white plates. mp=32°-35° C. (lit. mp=35°-36° C.)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05599926 |
| 出典データセット | uspto-grants-1997_02 |
| ORD ID | ord-12855e9ebf6145e3baf125f73f8c0817 |
| 出典メモ | uspto-grants-1997_02 |