反应详情

4-(3-Aminopropoxy)-6-chloro-1-benzopyran-2-one trifluoroacetate salt (0.272 mmol, 0.10 g) is suspended in 2 mL of DCM. DIEA (1.36 mmol, 0.236 mL) is added followed by methanesulfonyl chloride (0.543 mmol, 0.062 g) and the reaction is stirred at ambient temperature for 4 hrs. The solvent is removed under reduced pressure and the residue is redissolved and purified by HPLC to afford the title compound (21 mg, 23%); 1H NMR (DMSO-d6, 300 MHz) δ 7.80 (1H, d, J=2.6 Hz), 7.70 (1H, dd, J=2.5, 8.75 Hz), 7.45 (1H, d, J=8.87 Hz), 7.11 (1H, brt), 5.97 (1H, s), 4.28 (2H, t, J=6 Hz), 3.16 (2H, m), 2.91 (3H, s), 2.01 (2H, m); MS (ESI, Pos.) calcd for C13H14ClNO5S m/z [M+H]=332.0, found 331.9.

1. customThe solvent is removed under reduced pressure
2. dissolutionthe residue is redissolved
3. custompurified by HPLC