反应详情

A solution of the product from step (i) (3.14 g) and N-bromosuccinimide (2.18 g) in benzene (40 ml) was irradiated with a 500 Watt halogen lamp for 2 h. The reaction mixture was partitioned between dichloromethane and water. The organic phase was further washed with water, collected, dried (MgSO4) and solvent evaporated under reduced pressure. The residue was dissolved in dichloromethane (25 ml) and triethylamine (10 ml) added. After stirring for 16 h the solvent/reagent were evaporated under reduced pressure. Purification was by chromatography eluting with 30-40% ethyl acetate in isohexane.

1. customThe reaction mixture was partitioned between dichloromethane and water
2. washThe organic phase was further washed with water
3. customcollected
4. dry with materialdried (MgSO4) and solvent
5. customevaporated under reduced pressure
6. dissolutionThe residue was dissolved in dichloromethane (25 ml)
7. additiontriethylamine (10 ml) added
8. customwere evaporated under reduced pressure
9. customPurification
10. washeluting with 30-40% ethyl acetate in isohexane