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Hydrochloric Acid → 3-(4-Fluorophenyl)-5-isopropyl-1-(4-methylpiperidino)-2-phenyl-pyrrole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 4-Methylpiperidin-1-amine | HCID 3733587 | — |
| 反応物 | 2-(4-Fluorophenyl)-5-methyl-1-phenylhexane-1,4-dione | HCID 14300271 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-(4-Fluorophenyl)-5-isopropyl-1-(4-methylpiperidino)-2-phenyl-pyrrole | HCID 14578771 | — |
反応手順
3.4 ml of conc. hydrochloric acid are added to 10.1 g (34 mmol) of the compound from Example 2 and 11.6 g (102 mmol) of N-amino-4-methyl-piperidine in 100 ml of toluene AR and 50 ml of dimethylformamide and the mixture is boiled for 24 hours in a water separator. The mixture is cooled, diluted using 200 ml of ethyl acetate and extracted three times using 1N hydrochloric acid and twice using saturated sodium hydrogen carbonate solution. The organic phase is dried over magnesium sulphate and concentrated in vacuo, and the residue is chromatographed on a column (silica gel 70-230 mesh, using ethyl acetate/petroleum ether 5:95).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04988711 |
| 出典データセット | uspto-grants-1991_01 |
| ORD ID | ord-ded4a07d12c349e18f01b4b42b5ff57f |
| 出典メモ | uspto-grants-1991_01 |