反应详情

To a stirred solution of the intermediate from Step A in THF (50 mL) was added DABCO (1.51 g, 13.5 mmol) and then p-toluenesulfonyl chloride (50 mL). The resulting mixture was stirred overnight at room temperature and then filtered to remove precipitated hydrochloride salts. The filtrate was concentrated under reduced pressure and DCM (50 mL) was added to the residue. The organic layer was then washed with water (1×100 mL), saturated NaCl (1×100 mL), dried over magnesium sulfate, filtered and the solvent removed under reduced pressure. The resulting material was purified by silica gel chromatography (70% EtOAc/hexane) to afford 1.25 g of the title intermediate (43% yield).

1. filtrationfiltered
2. customto remove
3. customprecipitated hydrochloride salts
4. concentrationThe filtrate was concentrated under reduced pressure and DCM (50 mL)
5. additionwas added to the residue
6. washThe organic layer was then washed with water (1×100 mL), saturated NaCl (1×100 mL)
7. dry with materialdried over magnesium sulfate
8. filtrationfiltered
9. customthe solvent removed under reduced pressure
10. customThe resulting material was purified by silica gel chromatography (70% EtOAc/hexane)