反应详情

Intermediate 33 (0.377 g, 1.147 mmol) in 10 mL of TEA was combined with PdCl2(PPh3)2 (0.02294 mmol, 0.016 g) the mixture was then degassed using N2 for 5 minutes. Then CuI (0.01147 mmol, 0.002 g) and Pent-4-yn-1-ol (1.147 mmol, 0.115 g) then reacted at 50° C. for 4 hours. The reaction was worked up quenching the reaction with 1× saturated NaHCO3, extracted 4×25 ml EtOAc then washed 1× water, 1× saturated NaCl, dried over Na2SO4, then concentrated. The product was purified 0-75% EtOAc in Hexanes over 20 min on silica. ES/MS calcd. for C14H14F3NO2 285.1. Found m/z=286 (M+H)+.

1. customwas then degassed
2. customfor 5 minutes
3. customThe reaction was worked up quenching
4. customthe reaction with 1× saturated NaHCO3
5. extractionextracted 4×25 ml EtOAc
6. washthen washed 1× water, 1× saturated NaCl
7. dry with materialdried over Na2SO4
8. concentrationconcentrated
9. customThe product was purified 0-75% EtOAc in Hexanes over 20 min on silica