反应详情

A solution of Example 129C (1.0808 g, 3.52 mmol) in pyridine (17.5 mL) was treated with phenylsulfonyl chloride (0.58 mL, 4.58 mmol), stirred for 2 hours, diluted with CH2Cl2, washed with 1N HCl (3×50 mL) and brine (50 mL), dried (MgSO4), filtered, and concentrated. The residue was purified by flash column chromatography on silica gel with 9:1 hexanes/ethyl acetate to provide the desired product (450 mg, 35%); MS (ESI(+)) m/e 368 (M+H)+; MS (ESI(−)) m/e 364, 366 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 7.70 (m, 2H), 7.63 (m, 1H), 7.56 (m, 2H), 7.51 (m, 1H), 7.42 (m, 1H), 3.00 (m, 2H), 2.66 (m, 2H).

1. washwashed with 1N HCl (3×50 mL) and brine (50 mL)
2. dry with materialdried (MgSO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by flash column chromatography on silica gel with 9:1 hexanes/ethyl acetate