反应详情

1.8 g (5.4 mmol) of 2-(4-tert-butyl-2-1,3-dioxinan-2-yl-6-fluoro-phenyl)-4,4-dimethyl-4,5-dihydro-oxazole was weighed into a 200 mL round bottom flask fitted with a stir bar and reflux condenser. Added 75 mL of ethanol and stirred to obtain a clear solution. Added 50 mL of 50% aqueous sulfuric acid. Stirred at reflux for 18 h. Poured the reaction mixture into 400 mL water. Extracted the aqueous mixture with 2×200 mL CH2Cl2. Combined the organic extracts and washed with 200 mL brine. Dried over Na2SO4 and removed the solvent on rotavap. Dried under high vacuum to obtain 1.29 g of the title compound as on off-white solid. MS (ESI) 223 (M−H)−.

1. customfitted with a stir bar
2. temperaturereflux condenser
3. customto obtain a clear solution
4. stirringStirred
5. temperatureat reflux for 18 h
6. extractionExtracted the aqueous mixture with 2×200 mL CH2Cl2
7. washwashed with 200 mL brine
8. dry with materialDried over Na2SO4
9. customremoved the solvent on rotavap
10. customDried under high vacuum