Sodium Hydroxide → HCID 11457378, compound

Participants

Reaction Conditions

Reaction Steps

1.0M Sodium hydroxide solution (26.3 ml) was added to a stirred solution of methylammonium (E)-7-[4-(4-fluorophenyl)-6-isopropyl-2-[methyl(methylsulfonyl)amino]-pyrimidin-5-yl]-(3R,5S)-3,5-dihydroxyhept-6-enoate (15 g) in water (106 ml) at ambient temperature. A solution of magnesium sulphate (4.3 g) in water (26 ml) was added over 20 minutes and a solid precipitated. The solid was collected by filtration, washed with water (20 ml) and dried under vacuum at 40° C. (7.7 g). A mixture of the solid (5.8 g) and water (50 ml) was heated to 38° C. and diluted with water (35 ml). The mixture was stirred at ambient temperature for 4 hours and then allowed to stand for 66 hours. The solid was collected by filtration after diluting with water (30 ml). The product was dried at 35° C. under vacuum to give magnesium (E)-7-[4-(4-fluorophenyl)-6-isopropyl-2-[methyl(methylsulfonyl)amino]-pyrimidin-5-yl]-(3R,5S)-3,5-dihydroxyhept-6-enoate (4.68 g) as white crystals. The X-ray powder diffraction spectra for a typical sample of the crystalline magnesium salt is shown in FIG. 9 hereinafter. The ten most prominent peaks in the XRD occur at about 2-theta=11.5, 14.5, 16.3, 16.8, 18.0, 19.1, 19.8, 21.8, 22.6 and 23.0°.

Provenance & Evidence