反应详情

In this example, 26.1 g of methyl 11-(3-dimethylaminopropylidene)-6,11-dihydrodibenz[b,e]oxepin-2-carboxylate is dissolved in a mixed solvent of 500 ml of methanol and 30 ml of water and 6.2 g of sodium hydroxide is added thereto. The mixture is heated at reflux for two hours. After allowing the mixture to stand for cooling, aqueous 4N-hydrochloric acid solution is added thereto to adjust the pH to 7 and the mixture is concentrated under reduced pressure. The concentrate is purified by column chromatography on high porous polymer (HP-20) (eluent: water:methanol=1:2) to obtain 25.0 g of the desired product.

1. additionis added
2. temperatureThe mixture is heated
3. temperatureat reflux for two hours
4. temperaturefor cooling
5. concentrationthe mixture is concentrated under reduced pressure
6. customThe concentrate is purified by column chromatography on high porous polymer (HP-20) (eluent: water:methanol=1:2)