反应详情

The compound of step 1 of example 252 (20 g, 89.2 mmol) was dissolved in DMF (100 ml) and cooled in an ice bath. Potassium carbonate (18.4 g, 134 mmol) and, immediately thereafter, benzyl bromide (15.2 g, 89.2 mmol) were added. The mixture was stirred for 30 min at room temperature, filtered into a mixture of 2 N hydrochloric acid and diethyl ether. The solid was washed repeatedly with diethyl ether. The combined ethereal phases were washed with water, dried over sodium chloride, decanted and evaporated to dryness. The residue was purified by silica gel chromatography (HEP/EA gradient) to yield 21 g of the title compound.

1. temperaturecooled in an ice bath
2. filtrationfiltered into a mixture of 2 N hydrochloric acid and diethyl ether
3. washThe solid was washed repeatedly with diethyl ether
4. washThe combined ethereal phases were washed with water
5. dry with materialdried over sodium chloride
6. customdecanted
7. customevaporated to dryness
8. customThe residue was purified by silica gel chromatography (HEP/EA gradient)