Cl[CH2:2][C:3]1[N:8]=[C:7]([S:9][CH3:10])[N:6]=[C:5]([OH:11])[CH:4]=1.[Na+].[CH3:13][S:14]([O-:16])=[O:15].CN(C=O)C>C(#N)C>[CH3:10][S:9][C:7]1[N:6]=[C:5]([OH:11])[CH:4]=[C:3]([CH2:2][S:14]([CH3:13])(=[O:16])=[O:15])[N:8]=16-(Chloromethyl)-2-methylsulfanyl-pyrimidin-4-ol (19.07 g, 100 mmol) was suspended in acetonitrile (400 ml). To this stirring suspension was added methanesulphinic acid sodium salt (12.255 g, 120 mmol) and DMF (100 ml). The reaction was then heated to 100° C. to give a dark suspension and monitored by LCMS. Once complete, the solvents were removed and the resultant product added to 1:1 MeOH:DCM (200 ml) and acidified with acetic acid (10 ml). The resultant precipitate was collected, washed with water (200 ml) and MeOH (100 ml) and dried overnight in vacuo to afford the title compound as a white solid, 16.45 g.
Wird geladen…
