反应详情

温度

-78 °C

The product from Example 88C (0.983 g, 3.80 mmoles) in anhydrous THF (10 mL) at −78° C. was treated dropwise with 1.7 M t-butyllithium (4.46 mL, 7.59 mmoles). Reaction stirred 30 minutes at −78° C. and was then treated with the product from Example 88B (1.00 g, 1.90 mmoles. Reaction stirred 15 minutes at −78° C. and then allowed to warm to 0° C. Reaction quenched with saturated NH4Cl and warmed to room temperature. The mixture was diluted with ethyl acetate, washed with H2O, brine, dried (Na2SO4), filtered, and the filtrate concentrated under reduced pressure. The residue was purified by chromatography on a pre-packed Biotage silica gel column (30% ethyl acetate:hexanes) to provide the title compound (0.369 g, 36%). MS (ESI−) m/z 539 (M−H)−.

1. customReaction
2. customReaction
3. stirringstirred 15 minutes at −78° C.
4. temperatureto warm to 0° C
5. customReaction
6. customquenched with saturated NH4Cl
7. temperaturewarmed to room temperature
8. additionThe mixture was diluted with ethyl acetate
9. washwashed with H2O, brine
10. dry with materialdried (Na2SO4)
11. filtrationfiltered
12. concentrationthe filtrate concentrated under reduced pressure
13. customThe residue was purified by chromatography on a pre-packed Biotage silica gel column (30% ethyl acetate:hexanes)