反应详情

To a solution of t-BuOK (0.36 g, 3.2 mmol) in t-BuOH (10 mL) was added N-(2-(5-bromo-2-fluorophenyl)-3,3-difluoro-4-hydroxybutan-2-yl)-2-chloroacetamide (1.0 g, 2.6 mmol) t-BuOH (10 mL) at rt and heated to reflux temperature for 1 h 30 min. Reaction mixture was monitored by TLC analysis. Reaction mixture was concentrated under reduced pressure and adjusted pH to −2 using 2 N HCl. Ethyl acetate was added to extract the product, organic layer was washed with water, brine solution followed by drying over anhy. Na2SO4 and concentrated under reduced pressure. The crude compound (0.9 g) was carried forward for the next step without purification. LCMS: RtH8=1.616 [M+H]+=337.8, 339.9 (56%); 1.482 [M+H]+=675.1, 676.8 (34%).

1. temperatureheated
2. temperatureto reflux temperature for 1 h 30 min
3. customReaction mixture
4. customReaction mixture
5. concentrationwas concentrated under reduced pressure and adjusted pH to −2 using 2 N HCl
6. additionEthyl acetate was added
7. extractionto extract the product, organic layer
8. washwas washed with water, brine solution
9. customby drying over anhy
10. concentrationNa2SO4 and concentrated under reduced pressure
11. customThe crude compound (0.9 g) was carried forward for the next step without purification