反应详情

To a solution of Intermediate 2A (33.9 mg, 0.1 mmol) in DMF (Volume: 1 mL) under argon at room temp was added N-chlorosuccinimide (107 mg, 0.800 mmol). The reaction mixture was allowed to stir overnight. The reaction mixture was diluted with ethyl acetate and washed (2×15 mL) with 10% LiCl, once with brine, dried over Na2SO4, filtered and concentrated. The crude product was dissolved in a small amount of dichloromethane and charged to a 4 g silica gel cartridge which was eluted with a 20 min gradient from 0% to 100% of ethyl acetate in dichloromethane. The resulting brown solid (23 mg, 61.6%) was determined to be the desired material by 1HNMR and LCMS. MS (ES): m/z=274.0 [M+H]+. 1H NMR (400 MHz, CCl3D) δ ppm 8.58-8.60 (1 H, m), 8.24 (1 H, s), 8.14-8.20 (2 H, m), 7.18-7.26 (2 H, m).

1. washwashed (2×15 mL) with 10% LiCl
2. dry with materialonce with brine, dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. dissolutionThe crude product was dissolved in a small amount of dichloromethane
6. additioncharged to a 4 g silica gel cartridge which
7. washwas eluted with a 20 min gradient from 0% to 100% of ethyl acetate in dichloromethane