反应详情

To a solution of 11 (0.100 g, 0.225 mmol) in MeOH (5 ml), methanesulfonic acid (0.050 ml) was added and stirred at room temperature for 2 h. The solvents were removed under reduced pressure and acetone and ether were added. The solid was collected by filtration to give the product 12 (0.075 g, 52%). M.p. 258-268° C., 1H NMR (DMSO-d6, 500 MHz): δ 11.49 (1H, brs, NH), 10.25 (1H, brs, NH), 8.79 (1H, s), 8.165 (2H, d, J=9.0 Hz), 7.87 (2H, d, J=9.0 Hz), 8.78 (1H, s), 2.40 (6H, s), 2.37 (2H, m), 1.91-1.20 (20H, m); EIMS m/z: 541.1 (M+CH3SO3H), 446.5 (M+1); Anal. (C28H39N5O8S2×2.20H2O) C, H, N, S

1. customThe solvents were removed under reduced pressure and acetone and ether
2. additionwere added
3. filtrationThe solid was collected by filtration