反应详情

To a magnetically stirred solution of 1.20 g (2.14 mmol) the product of Step A dissolved in 12 mL of THF was slowly added 3.2 mL of a 1.0 N solution (3.2 mmol) of lithium bis(trimethylsilylamide) in THF at 0° C. The reaction mixture was stirred for 30 min and allowed to warm to room temperature. The reaction mixture was then quenched by addition of excesss 10% aqueous NaHSO4 and extracted into EtOAc. The organic layer was separated, washed with water, dried (MgSO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with chloroform. Combination of the purified fractions and drying in vacuo afforded the title compound.

1. customat 0° C
2. customThe reaction mixture was then quenched by addition of excesss 10% aqueous NaHSO4
3. extractionextracted into EtOAc
4. customThe organic layer was separated
5. washwashed with water
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customevaporated
9. customThe residue was purified on a silica gel flash chromatography column
10. washeluted with chloroform
11. customCombination of the purified fractions and drying in vacuo