化工社化工社 化学情報印刷レポート · 研究参考用
Acetonitrile → HCID 18173258、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | 4-Bromophenol | HCID 7808 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1,4-Dichloro-2-butene, (2E)- | HCID 642197 | — |
| 生成物 | HCID 18173258 | HCID 18173258 | — |
反応手順
80 mmol (17.4 g) of caesium carbonate are added to a solution, cooled to 0° C., of 80 mmol (10 g) of trans-1,4-dichloro-2-butene and 53.3 mmol (9.23 g) of para-bromophenol in 500 ml of acetonitrile, and then the mixture is stirred at ambient temperature for 4 days. The mixture is hydrolysed with 250 ml of a saturated aqueous solution of ammonium chloride and then extracted with ethyl acetate. The organic phases are combined and washed with a saturated aqueous solution of sodium chloride and then dried over magnesium sulphate. After evaporation, the expected product is obtained following purification by chromatography on silica gel using a 98:2 petroleum ether/ethyl acetate mixture as eluant.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06605604B1 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-87d9bd6d6bf94b6d8f802cf54e916eb0 |
| 出典メモ | uspto-grants-2003_08 |