反应详情

To a mixture of 2,2-dimethylmalonic acid mono-t-butyl ester (10 g), 2,2-dimethyl-1-propanol [CAS No. 75-84-3] (5.15 g), DMAP (1.3 g), and dichloromethane (100 mL), WSC (12.2 g) was added with stirring under ice-cooling, and the resulting mixture was stirred at room temperature for 2 days. TBME and water were added to the mixture, and the resulting mixture was extracted. The organic layer was sequentially washed with water and saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The desiccant was filtered off, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was purified by silica gel column chromatography (mixed solvent of heptane-ethyl acetate) to obtain 2,2-dimethylmalonic acid t-butyl ester(2,2-dimethylpropyl)ester (12 g).

1. temperaturecooling
2. stirringthe resulting mixture was stirred at room temperature for 2 days
3. extractionthe resulting mixture was extracted
4. washThe organic layer was sequentially washed with water and saturated aqueous sodium chloride solution
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationThe desiccant was filtered off
7. customthe filtrate obtained
8. concentrationwas concentrated under reduced pressure
9. customThe residue obtained
10. customwas purified by silica gel column chromatography (mixed solvent of heptane-ethyl acetate)