化工社化工社 化学情報印刷レポート · 研究参考用
p-Toluenesulfonic acid → 7-Methoxy-spiro[1,3-benzodioxole-2,1'-cyclopentane]
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Cyclopentanone | HCID 8452 | — |
| 反応物 | 3-Methoxycatechol | HCID 13622 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Methylorthoformate | HCID 53629101 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 7-Methoxy-spiro[1,3-benzodioxole-2,1'-cyclopentane] | HCID 22734358 | — |
反応手順
A mixture of 3-methoxycatechol (22.6 g), cyclopentanone (27.1 g), methyl orthoformate (34.2 g), p-toluenesulfonic acid.monohydrate (0.2 g), and benzene (300 ml) was heated under reflux for 24 hours. After being allowed to stand for cooling, a dilute solution of sodium hydroxide was added to the mixture followed by extraction with ether. The organic layer was washed with a saturated saline and dried over anhydrous potassium carbonate. The solvent was distilled off under reduced pressure to give Compound IIax-a (30 g, 90%) as a colorless oily substance.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06716987B1 |
| 出典データセット | uspto-grants-2004_04 |
| ORD ID | ord-5538919769214dd8ac3ff1eea426cd8d |
| 出典メモ | uspto-grants-2004_04 |