反应详情

温度

55 °C

A mixture of 3,5-difluorophenol (TCl, 14 g, 107 mmol), tert-butyl methyl ether (12.8 ml, 108 mmol) and zirconium(IV) chloride (25 g, 107 mmol) was stirred for 12 hours at 55 ° C., followed by addition of tert-butyl methyl ether (6.4 ml, 54 mmol). The additional injection of tert-butyl methyl ether (6.4 ml, 54 mmol), was repeated 8 times at intervals of 24 hours and then the reaction was quenched with saturated ammonium chloride aqueous solution and 2 M HCl aqueous solution. The whole was extracted with DCM, washed with brine, and dried over magnesium sulfate. The organic layer was evaporated to give a crude residue which was purified by silica gel column chromatography, eluting with gradually from hexane only to hexane/EtOAc (10:1), to give the title compound (10.8 g, 54%) as white solids.

1. customat intervals of 24 hours
2. customthe reaction was quenched with saturated ammonium chloride aqueous solution and 2 M HCl aqueous solution
3. extractionThe whole was extracted with DCM
4. washwashed with brine
5. dry with materialdried over magnesium sulfate
6. customThe organic layer was evaporated
7. customto give a crude residue which
8. customwas purified by silica gel column chromatography
9. washeluting with gradually from hexane only to hexane/EtOAc (10:1)