反应详情

温度

0 °C

Sodium hydride, 60% dispersion (66 mg, 1.66 mmol), was rinsed with hexane, suspended in 7 mL of DMF and cooled to 0° C. To this suspension was added 2,4-difluorophenol (170 μL, 1.79 mmol). After 5 minutes at 0° C., 2-bromoacetic acid 2-methyl-1-(4-(methylsulfonyl)phenyl)propan-1-one ester (Step 1) (233 mg, 1.79 mmol) was added and the reaction mixture was stirred for 30 minutes. Dichloromethane was added and the mixture was washed with 1N HCl and the organic solvent was evaporated under vacuum. The residue was dissolved in 25%EtOAc/Et20 and washed with 1N NaOH, water (2×) brine and dried over MgSO4. After filtration and evaporation of the solvent under vacuum 470 mg of the title compound was obtained.

1. washSodium hydride, 60% dispersion (66 mg, 1.66 mmol), was rinsed with hexane
2. washthe mixture was washed with 1N HCl
3. customthe organic solvent was evaporated under vacuum
4. dissolutionThe residue was dissolved in 25%EtOAc/Et20
5. washwashed with 1N NaOH, water (2×) brine
6. dry with materialdried over MgSO4
7. filtrationAfter filtration and evaporation of the solvent under vacuum 470 mg of the title compound
8. customwas obtained