反应详情

To a solution of 1 g of product from Example 4 in 15 ml of dry tetrahydrofuran is added in one portion 0.0622 g of sodium hydride. The mixture is heated at reflux temperature for 2 hours, cooled to room temperature and 0.442 g o-anisoyl chloride is added. The reaction is then heated at reflux for 1.5 hours, cooled to room temperature, poured into water and extracted with ethyl acetate. The organic layer is washed with saturated sodium chloride, dried and concentrated in vacuo. The residue is purified by column chromatography (silica gel: 35% ethyl acetate/hexane) to give 1.27 g of the desired product.

1. temperatureThe mixture is heated
2. temperatureat reflux temperature for 2 hours
3. temperatureThe reaction is then heated
4. temperatureat reflux for 1.5 hours
5. temperaturecooled to room temperature
6. extractionextracted with ethyl acetate
7. washThe organic layer is washed with saturated sodium chloride
8. customdried
9. concentrationconcentrated in vacuo
10. customThe residue is purified by column chromatography (silica gel: 35% ethyl acetate/hexane)