反应详情

To a solution of compound 30 (3.50 g, 12.9 mmol) and 4-methoxybenzyl trichloroacetimidate (4.65 g, 17.3 mmol) in DCM (100 mL) was added camphorsulfonic acid (450 mg, 1.92 mmol). The mixture was stirred overnight at room temperature. The mixture was washed with a saturated solution of NaHCO3 (300 mL) and water (300 mL) and dried over Na2SO4. The drying agent was removed by filtration and the solvents removed using a rotary evaporator. The residue was purified by chromatography on silica gel (120 g RediSep column, eluting with a gradient of 0% through 30% ethyl acetate/hexanes over 70 min, 85 mL/min) to give the product 32 (4.01 g, 81%) as a colorless liquid.

1. washThe mixture was washed with a saturated solution of NaHCO3 (300 mL) and water (300 mL)
2. dry with materialdried over Na2SO4
3. customThe drying agent was removed by filtration
4. customthe solvents removed
5. customa rotary evaporator
6. customThe residue was purified by chromatography on silica gel (120 g RediSep column
7. washeluting with a gradient of 0% through 30% ethyl acetate/hexanes over 70 min