Magnesium Hydroxide → HCID 72700513, compound

Participants

Reaction Steps

To a suspension of ((5-(5-phenyl-4-((pyridin-2-ylmethyl)amino)quinazolin-2-yl)pyridin-3-yl)sulfonyl)phosphoramidic acid (2) (0.050 g, 0.091 mmol) in ethanol (5 mL) was added magnesium hydroxide (7.97 mg, 0.137 mmol) in 1 mL of water. The resulting mixture was stirred under nitrogen atmosphere at room temperature for 2 h. The reaction mixture was concentrated to dryness and the residue was washed with ethyl acetate (2×5 mL), acetone (2×10 mL) and acetonitrile (2×10 mL) to afford magnesium(5-(5-phenyl-4-((pyridin-2-ylmethyl)amino)quinazolin-2-yl)pyridin-3-yl)sulfonylphosphoramidate (8) (0.040 g, 0.069 mmol, 76% yield) as a yellow solid. 1H NMR was not taken because of poor solubility. LCMS Method I: retention time 1.66 min, [M−1]=547. HPLC Method B: Purity 98.1%, retention time 6.18 min, HPLC Method C: Purity 95.6%, retention time 5.98 min. Elemental analysis: MF C25H20N6SPO5.Mg H2O, Calculated C, 46.15; H, 4.41; N, 12.92; Mg, 4.15; H2O, 11.70. Found C, 40.66; H, 4.12; N, 11.23; Mg, 4.14; H2O, 11.70; C and N are not in agreement.

Provenance & Evidence