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Sodium Carbonate → 9-Hydroxy-7-(3-methyl-2-octyl)-2,2,-dimethyl-4-oxo-1,2,3,4-tetrahydrocyclopenta[c] [1]benzopyran
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 5-(3-Methyloctan-2-yl)benzene-1,3-diol | HCID 258176 | — |
| 反応物 | Ethyl 4,4-dimethyl-2-oxocyclopentane-1-carboxylate | HCID 11735559 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 9-Hydroxy-7-(3-methyl-2-octyl)-2,2,-dimethyl-4-oxo-1,2,3,4-tetrahydrocyclopenta[c] [1]benzopyran | HCID 54133853 | — |
反応手順
to 13.5 g. of 5-(3-methyl-2-octyl)-resorcinol and 10.5 g. of 4,4-dimethyl-2-carboethoxycyclopentanone [Canadian J. of Chem. 47, 1982-1988 (1969)] in 59 ml. of benzene was added 4.3 ml. of phosphorus oxychloride with stirring and refluxing for 6 hours. The red solution was let stand at room temperature for 8 hours, poured into ice and sodium carbonate solution. The colorless mixture was extracted with ether, dried over magnesium sulfate and concentrated. The mixture was extracted with cold pentane and the pentane was discarded. The residue [9-hydroxy-7-(3-methyl-2-octyl)-2,2-dimethyl-4-oxo-1,2,3,4-tetrahydrocyclopenta[ c][1]benzopyran] was obtained as a gummy solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03941782 |
| 出典データセット | uspto-grants-1976_03 |
| ORD ID | ord-11315d3d7c174797a95fe7c427770b3b |
| 出典メモ | uspto-grants-1976_03 |