反应详情

5-(5-Bromo-2-fluoro-phenyl)-5-difluoromethyl-morpholin-3-one (190 g, 586 mmol) [example 42 step e)] and sodium acetate (57.7 g, 703 mmol) were suspended in 1850 mL methanol. 10% Pd on charcoal (18.7 g) was then added and the reaction mixture was shaken in a Parr apparatus in an atmosphere of hydrogen at rt. After 60 minutes the reaction mixture was filtered over celite and evaporated. The residue was dissolved in 2 L TBME and washed with aqueous NaHCO3 and brine. The organic layer was dried over MgSO4.H2O and evaporated to give 143.2 g of the title compound as a white solid.

1. filtrationAfter 60 minutes the reaction mixture was filtered over celite
2. customevaporated
3. dissolutionThe residue was dissolved in 2 L TBME
4. washwashed with aqueous NaHCO3 and brine
5. dry with materialThe organic layer was dried over MgSO4.H2O
6. customevaporated