反应详情

Dissolve 1-((1S,3R)-3-(((tert-butyldimethylsilyl)oxy)methyl)-5-(2-hydroxyethyl)-1-methyl-3,4-dihydroisoquinolin-2(1H)-yl)-2-(2-chloro-6-fluorophenyl)ethan-1-one (1.08 g, 2.13 mmol) in CH2Cl2 (21 mL). Add NaHCO3 (1.08 g, 12.9 mmol) and 3,3,3-triacetoxy-3-iodophthalide (1.09 g, 2.56 mmol) at room temperature. Stir 40 min. Add saturated NaHCO3 solution and saturated Na2S2O3 solution, extract with ethyl acetate three times. Combine the ethyl acetate extracts, dry over sodium sulfate, filter, and concentrate under reduced pressure to give a residue. Purify the residue by silica gel chromatography, eluting with ethyl acetate: hexanes (gradient, 5-60%) to give the title compound as a white foam (0.87 g, 1.73 mmol).

1. customat room temperature
2. extractionAdd saturated NaHCO3 solution and saturated Na2S2O3 solution, extract with ethyl acetate three times
3. dry with materialdry over sodium sulfate
4. filtrationfilter
5. concentrationconcentrate under reduced pressure
6. customto give a residue
7. customPurify the residue by silica gel chromatography
8. washeluting with ethyl acetate