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Ethylene Glycol → 1-(3',4'-Dimethoxyphenyl)-7-(4'-fluorophenyl)-2-nitro-5-heptanone ethylene ketal
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 1-(3',4'-Dimethoxyphenyl)-7-(4'-fluorophenyl)-2-nitro-5-heptanone | HCID 20164210 | — |
| 溶媒 | Cyclohexane | HCID 8078 | — |
| 生成物 | 1-(3',4'-Dimethoxyphenyl)-7-(4'-fluorophenyl)-2-nitro-5-heptanone ethylene ketal | HCID 56626552 | — |
反応手順
Into a 1 l. r.b. flask equipped with a Dean-Stark trap was placed 79 g (0.2 mole) of 1-(3',4'-dimethoxyphenyl)-7-(4'-fluorophenyl)-2-nitro-5-heptanone, 38 g p-toluenesulfonic acid, 120 ml ethylene glycol and 400 ml cyclohexane. The mixture was allowed to reflux overnight, then concentrated in vacuo. Dil NaHCO3 solution was added to the residue and extracted with methylene chloride. The organic layer was backwashed with water, dried over anh MgSO4, filtered and concentrated under reduced pressure to obtain 84.8 g of oily product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04342692 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-bae0000642044e9ba37819f228b9598f |
| 出典メモ | uspto-grants-1982_08 |