反应详情

POCl3 (0.34 mL, 3.558 mmol) was added to a cooled solution of potassium 3-(benzyloxy)cyclobutane-1-sulfonate (0.5 g, 1.779 mmol) in dry DCM (10 mL) at 0° C. This was followed by the slow addition of diisopropyl ethyl amine (0.65 mL, 3.558 mmol) and stirred the resulting reaction mixture at 0° C. for 2 hours. The reaction was monitored by TLC (20% ethyl acetate in hexane). The reaction mixture was extracted with DCM. The organic layer was washed with water, brine solution, dried over Na2SO4 and concentrated. Purification by column chromatography on silica gel (8% ethyl acetate in hexane) afforded 0.15 g of the product (38% yield).

1. customthe resulting reaction mixture at 0° C. for 2 hours
2. extractionThe reaction mixture was extracted with DCM
3. washThe organic layer was washed with water, brine solution
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customPurification by column chromatography on silica gel (8% ethyl acetate in hexane)