反应详情

A solution of the product from step d) (4.04 g, 9.59 mmol) in CH2Cl2 (13.7 ml) was added dropwise to a slurry of AlCl3 (3.83 g, 28.77 mmol) in CH2Cl2 (36 ml) at 22° C. After 45 minutes, the reaction mixture was poured into ice cold 2 M NaOH (100 ml) and extracted with CH2Cl2 (300 ml). The organic layer was dried (MgSO4) and solvent evaporated in vacuo to give a residue that was purified by silica-gel chromatography using a ethyl acetate/hexanes gradient (0% to 50% ethyl acetate) to give the subtitle compound (2.4 g, 72%). MS calculated for C16H14BrNOS+H 348, observed 348, 350.

1. extractionextracted with CH2Cl2 (300 ml)
2. dry with materialThe organic layer was dried (MgSO4) and solvent
3. customevaporated in vacuo
4. customto give a residue that
5. customwas purified by silica-gel chromatography