反应详情

A solution of E-7-[2-(N-methyl-N-methanesulfonylamino)-4-(4-fluorophenyl)-6-isopropyl-pyrimidin-5-yl]-(3R,5S)-3,5-dihydroxyhept-6-enoic acid diisopropylamine salt (40.0 g) in a mixed solvent of ethyl acetate (400.0 mL) and water (400.0 mL) was cooled to 0˜5° C. The pH of the reaction mixture was adjusted to 3.0˜4.0 using 1N hydrochloric acid solution. Water (360.0 mL) was added to the separated organic layer, the pH of which was then adjusted to 9.0˜11.5 using 1N sodium hydroxide solution. Calcium chloride dihydrate (10.0 g) was added to the separated water layer. The reaction mixture was stirred at 20˜25° C. for 2 hours and then filtered under reduced pressure. The resulting white solid was dried to obtain E-7-[2-(N-methyl-N-methanesulfonylamino)-4-(4-fluorophenyl)-6-isopropyl-pyrimidin-5-yl]-(3R,5S)-3,5-dihydroxyhept-6-enoic acid 1/2 calcium salt (33.0 g, yield 95%, HPLC purity 99.7%).

1. filtrationfiltered under reduced pressure
2. customThe resulting white solid was dried