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3-Bromopropionitrile → 4-[alpha-(2-Pyridyl)benzyl]-1-(2-cyanoethyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Bromopropionitrile | HCID 17020 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1-[Phenyl(pyridin-2-yl)methyl]piperazine | HCID 3346446 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-[alpha-(2-Pyridyl)benzyl]-1-(2-cyanoethyl)piperazine | HCID 19370362 | 88% |
反応手順
1.05 g of N,N-diisopropyl-N-ethylamine was added, with stirring, to a solution of 2.0 g of 4-[α-(2-pyridyl)benzyl]piperazine and 1.0 g of 3-bromopropionitrile in 20 ml of methylene chloride, whilst ice-cooling, and the mixture was stirred at room temperature for 16 hours. At the end of this time, the mixture was poured into ice-water and extracted with chloroform. The extracts were combined and dried over anhydrous sodium sulfate, after which the solvent as removed by evaporation under reduced pressure. The resulting residue was purified by column chromatography through silica gel, using a 20:1 by volume mixture of ethyl acetate and ethanol as the eluent, to give 2:1 g (yield 88%) of the title compound as crystals, melting at 114°-116° 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-eb8b5e04c7ed4533942187c2f4999c2b |
| 出典メモ | uspto-grants-1995_11 |