反应详情

A solution of alcohol 5 (4.0 g, 17.9 mmol) and pyridine (10 ml, 6.9 equiv.) in CH2Cl2 (100 ml) was cooled in an ice bath and p-nitrophenyl chloroformate (5.42 g, 1.5 equiv.) was added. The resulting solution was stirred at RT for 16 h then washed with a 1 M HCl aqueous solution (3×50 ml), dried over MgSO4, filtrated then concentrated under reduced pressure. Purification by flash column chromatography (eluent: pet. ether/AcOEt 7:3 then 1:1) afforded carbonate 6 as a white amorphous solid (6.3 g, 91%).

1. washthen washed with a 1 M HCl aqueous solution (3×50 ml)
2. dry with materialdried over MgSO4
3. filtrationfiltrated
4. concentrationthen concentrated under reduced pressure
5. customPurification by flash column chromatography (eluent