反应详情

Diethylazodicarboxylate (0.6 mL, 3.84 mmol) was added to the solution of 160 (1.05 g, 2.75 mmol), 2-morpholinoethanol (0.5 mL, 3.84 mmol) and triphenylphosphine (1.01 g, 3.84 mmol) in tetrahydrofuran (27 mL). The reaction mixture was stirred until its completion, quenched with saturated aqueous ammonium chloride and extracted with EtOAc. The organic phase was washed with water and brine, dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The residue was purified by flash chromatography, eluent MeOH-DCM (2:98) to afford title compound 161 (906 mg, 66% yield) as a light-yellow solid. LRMS (M+1) 496.3 (100%).

1. customquenched with saturated aqueous ammonium chloride
2. extractionextracted with EtOAc
3. washThe organic phase was washed with water and brine
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. customevaporated under reduced pressure
7. customThe residue was purified by flash chromatography, eluent MeOH-DCM (2:98)