化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Carbonic acid, 2-methoxy-4-methylphenyl methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Methyl chloroformate | HCID 6586 | — |
| 反応物 | 2-Methoxy-4-Methylphenol | HCID 7144 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Carbonic acid, 2-methoxy-4-methylphenyl methyl ester | HCID 15636422 | 74.4% |
反応手順
2-methoxy-4-methylphenol (250 mmol) was dissolved in dry dichoromethane (500 ml) with pyridine (392 mmol) and DMAP (N,N-dimethyl-4-aminopyridine, 4.26 mmol). Methyl chloroformate (317 mmol) was added slowly to this solution and the reaction was stirred at room temperature for 3 hours. The reaction mixture was then poured onto a 2M HCl solution (120 ml), and the aqueous layer was extracted twice with dichloromethane (50 ml). Then the combined organic layers were washed twice with water (100 ml), dried over MgSO4 and filtered. The solvent was evaporated and the residue distilled under reduced pressure (120-140° C., 0.4 mbar) to give 38 g (186 mmol, 74% yield) of pure 2-methoxy-4-methyl-phenyl methyl carbonate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08648033B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-0f4f5e64b9c84451b283c4560e92bbb4 |
| 出典メモ | uspto-grants-2014_02 |