反应详情

A solution of compound 547 (3.2 g, 10.62 mmol) and AlMe3 (6.37 mL, 12.75 mmol) in DCM (40 mL) was stirred at 45° C. for 16 h and quenched with water. The reaction was diluted with AcOEt, washed with water and 1M HCl. The organic layer was separated, dried with Na2SO4, filtered and concentrated via rotary evaporation. The residue was triturated with AcOEt, filtered, washed with AcOEt and was purified via Isco employing a 0 to 50% AcOEt in hexanes solvent gradient to afford the title compound 548 (1.01 g, 35%) as a white solid.

1. customquenched with water
2. additionThe reaction was diluted with AcOEt
3. washwashed with water and 1M HCl
4. customThe organic layer was separated
5. dry with materialdried with Na2SO4
6. filtrationfiltered
7. concentrationconcentrated via rotary evaporation
8. customThe residue was triturated with AcOEt
9. filtrationfiltered
10. washwashed with AcOEt
11. customwas purified via Isco