反应详情

温度

80 °C

Intermediate 32 (1.0 g, 3.175 mmol) in 20 mL of acetone was combined with CH3I (6.350 mmol, 0.901 g, 0.395 mL) and K2CO3 (6.350 mmol, 0.876 g) then refluxed at 80° C. for 2 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 carried through without purification. ES/MS calcd. for C9H7F3INO 328.95. Found m/z=330 (M+H)+.

1. customThe reaction was worked up quenching
2. customthe reaction with 1× saturated NaHCO3
3. extractionextracted 4×25 mL EtOAc
4. washthen washed 1× water, 1× saturated NaCl
5. dry with materialdried over Na2SO4
6. concentrationconcentrated
7. customThe product was carried through without purification