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Hydrochloric Acid → 2-(3-Fluoro-4-methylphenyl)benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 4,5-Dihydro-5,5-dimethyl-2-(3'-fluoro-4'-methyl-biphenyl-2-yl)oxazole | HCID 54515599 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(3-Fluoro-4-methylphenyl)benzonitrile | HCID 54238624 | — |
反応手順
97.0 g (343 mmol) of the compound from Example III are initially introduced into 500 ml of pyridine, and 31.3 ml (343 mmol) of phosphorus oxychloride are added at 0° C., while stirring. The mixture is heated slowly, and is finally boiled under reflux for 1 hour. After cooling to room temperature, ether and an amount of 1M hydrochloric acid such that the pH of the aqueous phase is 1.5 are added. The organic phase is washed three more times with 1M sulphuric acid, dried with sodium sulphate and evaporated on a rotary evaporator and the residue is freed from the residual solvent under a high vacuum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05596006 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-03a275f73cc44f37bf751a999adad78a |
| 出典メモ | uspto-grants-1997_01 |