反应详情

A solution of Example 5F (50 mg. 0.16 mmole), pyridine (75 mg) and benzenesulfonyl chloride (86 mg., 0.5 mmole) in chloroform (1 mL) was stirred for 1 hour, washed with aqueous HCl (1M), dried (Na2SO4), filtered and concentrated under reduced pressure. The concentrate was purified by reverse-phase HPLC with CH3CN/water to provide the titled product. MS (ESI(−)Q1MS) m/z 442 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 10.38 (s, 1H), 8.22 (d, J=9 Hz, 1H), 7.70-7.50 (m, 5H), 7.36-7.29 (m, 3H), 7.16-7.06 (m, 4H), 6.76 (s, 1H), 6.69 (d, J=8 Hz, 1H), 6.62(d, J=8 Hz, 1H), 6.11 (s, 1H), 3.85 (s, 3H).

1. washwashed with aqueous HCl (1M)
2. dry with materialdried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe concentrate was purified by reverse-phase HPLC with CH3CN/water