反应详情

A solution of 1-Boc-3-azetidinone (800 mg, 4.67 mmol), 4-fluoro aniline (0.519 ml, 4.67 mmol), acetic acid (0.535 ml, 9.34 mmol) and sodium(triacetoxy)borohydride (1.98 g, 9.34 mmol) in 1,2-dichloroethane (20 ml) was stirred under N2 atmosphere at room temperature for 1 day. Sat. solution of NaHCO3 (25 ml) was added. After phase separation, the aqueous layer was extracted with dichloromethane (2×35 ml). The collected organics after solvent evaporation were purified by Biotage SNAP-Si cartridge (25 g) eluting with cyclohexane/ethylacetate from 90/10 to 80/20. Collected fractions after solvent evaporation afforded the title compound (D30) (880 mg)

1. customAfter phase separation
2. extractionthe aqueous layer was extracted with dichloromethane (2×35 ml)
3. customThe collected organics after solvent evaporation
4. customwere purified by Biotage SNAP-Si cartridge (25 g)
5. washeluting with cyclohexane/ethylacetate from 90/10 to 80/20
6. customCollected fractions after solvent evaporation