反应详情

A mixture of 2.0 g of the product of Step 5, 0.54 g of PdCl2dppf.CH2Cl2, and 1.8 ml of Et3N in 60 ml of 2:1 DMSO/MeOH was heated under CO (balloon pressure) at 75° C. for 24 h. The reaction mixture was poured into 400 ml of 1:1 heaxan/EtOAc and stirred with 200 ml of water for 4 h. The organic layer was washed with 100 ml of brine and dried over Na2SO4, filtered, and concentrated. The residue was purified by silica gel chromatography eluted with a gradient up to 15% EtOAc/hexane to give 1.7 g of the title compound as a light brown solid.

1. washThe organic layer was washed with 100 ml of brine
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by silica gel chromatography
6. washeluted with a gradient up to 15% EtOAc/hexane