反应详情

5.2 g of Ethyl 2-(diethylphosphoryl)-2-isopropylacetate was dissolved in 40 ml of tetrahydrofuran, and 0.53 g of 60% sodium hydride was added under ice-cooling, and the mixture was stirred for 20 minutes under ice-cooling. The reaction solution was treated with a solution of 3.0 g of 4-benzyloxybenzaldehyde in 15 ml of tetrahydrofuran and 10 ml of N,N-dimethylformamide, and stirred at room temperature for 16 hours. The reaction solution was diluted with water, and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and evaporated. The residue was subjected to silica gel column chromatography, and the fraction eluting with 5% ethyl acetate-hexane was concentrated. The residue was dissolved in 40 ml of ethanol, and 0.4g of 10% palladium carbon was added, the atmosphere was replaced with hydrogen, and the mixture was stirred at room temperature for 5 hours. Then, the atmosphere was replaced with nitrogen, the catalyst was filtered off, and the solvent was evaporated. The residue was subjected to silica gel column chromatography (20% ethyl acetate-hexane), to give 2.7 g of the title compound.

1. temperaturecooling
2. temperaturecooling
3. stirringstirred at room temperature for 16 hours
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with saturated brine
6. dry with materialdried over anhydrous magnesium sulfate
7. customevaporated
8. washthe fraction eluting with 5% ethyl acetate-hexane
9. concentrationwas concentrated
10. dissolutionThe residue was dissolved in 40 ml of ethanol
11. addition0.4g of 10% palladium carbon was added
12. stirringthe mixture was stirred at room temperature for 5 hours
13. filtrationthe catalyst was filtered off
14. customthe solvent was evaporated