反应详情

温度

40 °C

(E)-7-[4-(4-Fluorophenyl)-6-isopropyl-2-[methyl(methylsulfonyl)amino]pyrimidin-5-yl](3R,5S)-3,5-dihydroxyhept-6-enoic acid TRIS salt (17.7 g) was dissolved in degassed water (120 ml) at 20° C. then the solution was heated to 40° C. A solution of calcium chloride dihydrate (2.6 g) in water (25 ml) was added dropwise at about 40° C. over 20 minutes. The mixture was stirred for 15 minutes, allowed to cool to 20° C. over 60 minutes, held at this temperature for a further 60 minutes and the resultant solid filtered. The solid was washed with water (140 ml) and dried under a flow of nitrogen to give non-crystalline calcium salt of (E)-7-[4-(4-fluorophenyl)-6-isopropyl-2-[methyl(methylsulfonyl)amino]pyrimidin-5-yl](3R,5S)-3,5-dihydroxyhept-6-enoic acid.

1. temperatureto cool to 20° C. over 60 minutes
2. waitheld at this temperature for a further 60 minutes
3. filtrationthe resultant solid filtered
4. washThe solid was washed with water (140 ml)
5. customdried under a flow of nitrogen