反应详情

A mixture of Example 108B (576 mg, 2.2 mmol), anhydrous dichloromethane (22 mL), pyridine (0.4 mL) and benzenesulfonyl chloride (0.33 mL) was stirred 18 hours under nitrogen atmosphere. The mixture was concentrated, dissolved in ethyl acetate (100 mL), washed with 0.5M HCl (3×50 mL) and brine, dried (Na2SO4), filtered, concentrated, and purified on silica gel (20 g) with 50% dichloromethane in hexanes to provide the desired product. MS (ESI(+)) m/e 407 (M+H)+, 424 (M+NH4)+, 429 (M+Na)+; (ESI(−)) m/e 405 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 10.59 (br s, 1H), 7.77 (m, 3H), 7.64 (m, 1H), 7.56-7.37 (m, 7H), 7.24 (d, 1H), 5.31 (s, 2H), 2.32 (s, 3H).

1. concentrationThe mixture was concentrated
2. dissolutiondissolved in ethyl acetate (100 mL)
3. washwashed with 0.5M HCl (3×50 mL) and brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated
7. custompurified on silica gel (20 g) with 50% dichloromethane in hexanes