化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Carbonate → 4-Diphenylmethyl-1-(3-phthalimidopropyl)piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | N-3-Bromopropylphthalimide | HCID 21611 | — |
| 反応物 | 4-Benzhydrylpiperidine | HCID 88278 | — |
| 触媒 | Sodium Iodide | HCID 5238 | — |
| 溶媒 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 生成物 | 4-Diphenylmethyl-1-(3-phthalimidopropyl)piperidine | HCID 19370298 | 95.5% |
反応手順
A mixture of 1.8 g of 4-diphenylmethylpiperidine, 1.92 g of N-(3-bromopropyl)phthalimide, 3.0 g of sodium carbonate and 20 mg of sodium iodide in 70 ml of methyl isobutyl ketone was heated under reflux for 5 hours. At the end of this time, the mixture was cooled to room temperature and filtered. The filtrate was concentrated by evaporation under reduced pressure, and the resulting residue was purified by column chromatography through silica gel, using a 1:1 by volume mixture of hexane and ethyl acetate as the eluent, to give 3.0 g (yield 95%) of the title compound as crystals, melting at 104°-106° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05470851 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-c0475da7b76846b6ba4781be5221c883 |
| 出典メモ | uspto-grants-1995_11 |