反应详情

To a Smith PROCESS VIAL™ (2-5 ml) charged with a magnetic stirring bar, tert-butyl-2-bromo-1-(2-{(2-bromo-5-chlorobenzyl)[2-(dimethylamino)ethyl]amino}-2-oxoethyl)-3-cyclohexyl-1H-indole-6-carboxylate (from Step 8, 1 eq) in DMF dry (0.02 M), 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi-1,3,2-dioxaborolane (1.1 eq), PdCl2(dppf) (0.03 eq) and potassium acetate (3 eq) were added. The vial was closed with its cap and filled with N2 and microwaved in a Smith PERSONAL SYNTHESIZER at 150° C. for 6 min. The solution was then diluted with EtOAc, washed with H2O and brine, dried over Na2SO4, filtered and concentrated in vacuo to afford the crude that was filtered through a plug of silica (EtOAc:PE:Et3N) (5:5:0.1%) and used in the next step without further purification; MS (ES+) m/z 550 (M+H)+.

1. additionTo a Smith PROCESS VIAL™ (2-5 ml) charged with a magnetic stirring bar
2. additionwere added
3. customThe vial was closed with its
4. customcap
5. custommicrowaved in a Smith PERSONAL SYNTHESIZER at 150° C. for 6 min
6. washwashed with H2O and brine
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated in vacuo
10. customto afford the crude that
11. filtrationwas filtered through a plug of silica (EtOAc:PE:Et3N) (5:5:0.1%)
12. customused in the next step without further purification