反应详情

Methanesulfonic acid (54 mg, 0.5 mmol) was added to a solution of compound 4-(4-(imidazo[1,2-b]pyridazin-6-ylmethoxy)phenyl)-5-(4-methoxyphenyl)-2,2-dimethylfuran-3(2H)-one (250 mg, 0.5 mmol) in DCM (2 ml) and diethyl ether (20 mL) at RT under an atmosphere of nitrogen. The reaction mixture was stirred at RT for 4 h upon which the mixture was filtered and the solids were washed with 20% DCM in diethyl ether and dried in vacuo to afford 4-(4-(imidazo[1,2-b]pyridazin-6-ylmethoxy)phenyl)-5-(4-methoxyphenyl)-2,2-dimethylfuran-3(2H)-one methanesulfonate (240 mg, 80.0%,) as an off-white solid. 1H NMR: 200 MHz, DMSO-d6: δ 8.55 (s, 1H), 8.35 (d, 1H), 78.1 (s, 1H), 7.65 (d, 2H), 7.4 (d, 1H), 7.2 (d, 2H), 7.1 (d, 2H), 7.0 (d, 2H), 5.35 (s, 2H) 3.9 (s, 3H), 2.35 (s, 3H), 1.45 (s, 6H). HPLC: (98.3%, Condition-A).

1. filtrationwas filtered
2. washthe solids were washed with 20% DCM in diethyl ether
3. customdried in vacuo