反应详情

To a cold (0° C.), stirred solution of 1.05 g of N-(4-chlorobenzyl)-2-formyl-3-[(2-methoxyethoxy)methyl]-4-methyl-7-oxo-4,7-dihydrothieno[3,2-b]pyridine-6-carboxamide in 20 mL of CH2Cl2 is added 0.67 mL of acetic acid and 1.5 g of sodium triacetoxyborohydride. The mixture is allowed to warm to room temperature and stirred for 2 h, then partitioned between CH2Cl2 and aqueous NaHCO3. The organic phase is dried (Na2SO4) and concentrated under reduced pressure. Flash chromatography of the residue on silica using 2.5-4% MeOH in CH2Cl2 affords 1.08 g (100%) of the title compound as a yellow crystalline solid. Recrystallization from acetonitrile affords white spars.

1. custompartitioned between CH2Cl2 and aqueous NaHCO3
2. dry with materialThe organic phase is dried (Na2SO4)
3. concentrationconcentrated under reduced pressure