反应详情

Ethyl difluoroacetate (4.06 g, 32.7 mmol) was dissolved in methyl tert-butyl ether (50 mL). To the stirred solution was added 25 weight % sodium methoxide (7.07 g, 32.7 mmol) followed by 3′-fluoro-4′-methoxyacetophenone from Step 1 (5.0 g, 29.7 mmol). After stirring for 16 hours, 1N HCl (50 mL) was added. The organic layer was collected and washed with water (2×50 mL), dried over anhydrous MgSO4, filtered, and added to hexanes to precipitate a tan solid (7.0 g, 96%): mp 70–72° C.

1. customThe organic layer was collected
2. washwashed with water (2×50 mL)
3. dry with materialdried over anhydrous MgSO4
4. filtrationfiltered
5. additionadded to hexanes
6. customto precipitate a tan solid (7.0 g, 96%)