反应详情

温度

100 °C

20.0 g of 3-phenoxybenzyl 2-(3-chloro-4-hydroxyphenyl)-2-methylpropyl ether prepared in the above step (1), 2.67 g of 95% sodium hydroxide and 1.0 g of 5% Pd-C (50% hydrous) were added to 100 ml of 80% methanol and the mixture was stirred at 100° C. under a hydrogen pressure of 20 to 30 kg/cm2G for 6 h. After cooling, the catalyst was removed by filtration and the catalyst was washed thoroughly with benzene. The solvent was distilled off under reduced pressure. A dilute aqueous hydrochloric acid solution was added to the distillation residue. After extraction with benzene, the benzene solution was washed with water and dried. Benzene was distilled off under reduced pressure to obtain 18.2 g of intended 3-phenoxybenzyl 2-(4-hydroxyphenyl)-2-methylpropyl ether (m.p. 69.2° to 70.0° C.).

1. temperatureAfter cooling
2. customthe catalyst was removed by filtration
3. washthe catalyst was washed thoroughly with benzene
4. distillationThe solvent was distilled off under reduced pressure
5. additionA dilute aqueous hydrochloric acid solution was added to the distillation residue
6. extractionAfter extraction with benzene
7. washthe benzene solution was washed with water
8. customdried
9. distillationBenzene was distilled off under reduced pressure