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Sulfuric Acid → 5-Amino-2,2,4,6,7-pentamethyl-2,3-dihydrobenzofuran hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Methallyl alcohol | HCID 10557 | — |
| 反応物 | 4-Amino-2,3,5-trimethylphenol | HCID 11105537 | — |
| 生成物 | 5-Amino-2,2,4,6,7-pentamethyl-2,3-dihydrobenzofuran hydrochloride | HCID 10220422 | 14.4% |
反応手順
4-Amino-2,3,5-trimethylphenol (2.0 g, 13.2 mmol) and 2-methyl-2-propenol (1.15 g, 15.8 g) were heated under reflux in dichloromethane (20 ml) together with sulfuric acid (2 ml) for 18 hours. The reaction mixture was washed with aqueous saturated sodium bicarbonate solution, dried and then concentrated. The residue was purified by silica gel column chromatography (isopropyl ether). The purified product was converted into its hydrochloride and it was crystallized from ethanol-isopropyl ether to obtain the desired compound (460 mg, yield: 14.4%), m.p. 248°-250° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05594154 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-9c85de5899764bb1962a3d0000aeae6c |
| 出典メモ | uspto-grants-1997_01 |