反应详情

(R)-Methyl 4-azido-3,4-dihydro-2H-chromene-7-carboxylate (21.50 mmol, 1.0 eq) in 50 mL THF was cooled to 0° C., and treated with DIBAL (63.0 mmol, 3.0 eq). After 2.5 h, the reaction mixture was quenched by adding 50% saturated K—Na tartrate (60 mL). After stirring 1 h at room temperature, the solution was extracted with DCM (4×50 mL). The organic layers were then washed with water (2×50 mL), dried over MgSO4 and concentrated. The residue was purified using SiO2 chromatography (10→80% EtOAc/Hexanes) to afford the title compound.

1. customthe reaction mixture was quenched
2. additionby adding 50% saturated K—Na tartrate (60 mL)
3. extractionthe solution was extracted with DCM (4×50 mL)
4. washThe organic layers were then washed with water (2×50 mL)
5. dry with materialdried over MgSO4
6. concentrationconcentrated
7. customThe residue was purified