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5-(3-Methyloctan-2-yl)benzene-1,3-diol → 1,2-Dihydro-9-hydroxy-2-methyl-7-(3-methyl-2-octyl)-4-oxo-4H-thieno-[2,3-c][1]benzopyran
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5-(3-Methyloctan-2-yl)benzene-1,3-diol | HCID 258176 | — |
| 反応物 | Ethyl 5-methyl-3-oxo-tetrahydrothiophene-2-carboxylate | HCID 12716255 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1,2-Dihydro-9-hydroxy-2-methyl-7-(3-methyl-2-octyl)-4-oxo-4H-thieno-[2,3-c][1]benzopyran | HCID 21519988 | — |
反応手順
To 45 ml. of ethanol was added 8.8 g. of crude ethyl 5-methyl-3-oxo-tetrahydrothiophene-2-carboxylate and 5 g. of 5-(3-methyl-2-octyl) resorcinol. The mixture was cooled in ice and hydrogen chloride was bubbled in for onehalf hour. The mixture was stoppered and let stand at room temperature for 3 days. The reaction mixture was concentrated and dissolved in ether. The ether solution was extracted twice with water and once with aqueous sodium bicarbonate solution. The solution was dried over magnesium sulfate and concentrated. The product was crystallized from acetonitrile to give 4.65 g., m.p. 146°-149°C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03946111 |
| 出典データセット | uspto-grants-1976_03 |
| ORD ID | ord-4223cd0c4d2048bead90edbf766604c8 |
| 出典メモ | uspto-grants-1976_03 |