反应详情

温度

-78 °C

tert-Butyl 5-(tert-butyldiphenylsilanyloxy)-3-methoxymethylcarbamoylvalerate (4.61 g) and tetrahydrofuran (60 mL) were mixed. To the mixture was added dropwise diisobutylaluminum hydride (1.0 M in toluene) (13.1 mL) at −78° C. The mixture was stirred at −78° C. for 1.5 hr. To the mixture was added dropwise acetic acid (0.515 mL). After an addition of aqueous Rochelle salt at −20° C., the mixture was extracted with ethyl acetate. The organic layer washed with water, then dried over magnesium sulfate. The magnesium sulfate was filtered off and the filtrate was concentrated in vacuo. The resultant residue was purified by silica gel column chromatography (Eluent: ethyl acetate/hexane=1/25) to give the title compound (2.60 g).

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer washed with water
3. dry with materialdried over magnesium sulfate
4. filtrationThe magnesium sulfate was filtered off
5. concentrationthe filtrate was concentrated in vacuo
6. customThe resultant residue was purified by silica gel column chromatography (Eluent: ethyl acetate/hexane=1/25)