反应详情

To a solution of 0.183 g (0.5 mmol) of the product of Step B in 10 mL of methanol was added 0.1 g of 10% palladium on carbon catalyst and the reaction mixture was stirred in Parr shaker under 40 psig of hydrogen overnight. The reaction mixture was then filtered through Celite filter aid and the filtrate was evaporated in vacuo. The residue was purified on a silica gel flash chromatography column eluted with mixtures of CH2Cl2/MeOH/conc. NH4OH of the following compositions: 97/3/0.3; 95/5/0.5; and 90/10/1. Combination of the purified fractions and drying in vacuo afforded the title compound.

1. filtrationThe reaction mixture was then filtered through Celite
2. filtrationfilter aid
3. customthe filtrate was evaporated in vacuo
4. customThe residue was purified on a silica gel flash chromatography column
5. washeluted with mixtures of CH2Cl2/MeOH/conc
6. customCombination of the purified fractions and drying in vacuo