反应详情

To a stirred solution of cerium(III) chloride heptahydrate (6.36 g, 17.07 mmol) and (S)-tert-butyl 2-((tert-butyldimethylsilyloxy)methyl)-3-methyl-5-oxo-5,6-dihydropyridine-1(2H)-carboxylate (Intermediate 78, 6.07 g, 17.07 mmol) in MeOH (100 mL) at 0° C., sodium tetrahydroborate (0.646 g, 17.07 mmol) was added as a solid. The mixture was stirred at ambient temp for 1 h. The mixture was concentrated and diluted with NH4Cl(aq), H2O and extracted with ether. The ether layer was separated and washed with brine, dried over Na2SO4, filtered and concentrated to give the desired product (5.48 g, 90%) as a yellow oil.

1. concentrationThe mixture was concentrated
2. additiondiluted with NH4Cl(aq), H2O
3. extractionextracted with ether
4. customThe ether layer was separated
5. washwashed with brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated