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Pyridine-2-acetonitrile → 2-(2-Pyridyl)-3-(3,5-di-tert-butylphenyl)-2-propenenitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine-2-acetonitrile | HCID 75959 | — |
| 反応物 | 3,5-Bis(tert-butyl)benzaldehyde | HCID 1268253 | — |
| 触媒 | Piperidine | HCID 8082 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-(2-Pyridyl)-3-(3,5-di-tert-butylphenyl)-2-propenenitrile | HCID 53716171 | — |
反応手順
To a stirred solution of 2.0 g (9.17 mmole) 3,5-di-tertbutylbenzaldehyde in 75 ml absolute ethanol are added 1.19 g (10.1 mmole) 2-pyridylacetonitrile and 12 drops piperidine. The reaction flask is equipped with a condenser and a drying tube (using anhydrous CaSO4), and the reaction is stirred and heated. After refluxing for 8 hours, the reaction is allowed to cool to room temperature and stirred overnight for 16 hours. The solvent is removed by rotary evaporation, and the residue purified by flash chromatography on silica gel, eluting with hexane-ethyl acetate, 98:2. The colorless solid is washed with cold ether-hexane to give 2-(2-pyridyl)-3-(3,5-di-tert-butylphenyl)-2-propenenitrile, m.p. 90°-93° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05597837 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-08a056f471524fe5ba1ae4ecc0082ddb |
| 出典メモ | uspto-grants-1997_01 |