[OH-].[Na+].[OH:3][C:4]1[C:9]([NH:10][C:11](=[O:22])[C:12]2[CH:17]=[C:16]([CH3:18])[C:15]([O:19][CH3:20])=[C:14]([CH3:21])[CH:13]=2)=[C:8]([OH:23])[N:7]=[C:6]([S-:24])[N:5]=1.[Na+].I[CH3:27].Cl>O.CN1CCCC1=O>[OH:23][C:8]1[C:9]([NH:10][C:11](=[O:22])[C:12]2[CH:13]=[C:14]([CH3:21])[C:15]([O:19][CH3:20])=[C:16]([CH3:18])[CH:17]=2)=[C:4]([OH:3])[N:5]=[C:6]([S:24][CH3:27])[N:7]=122.78 g of sodium hydroxide were initially charged in 735 ml of water, the mixture was cooled to 0° C., 78.21 g of sodium 4,6-dihydroxy-5-(4-methoxy-3,5-dimethylbenzoylamino)pyrimidine-2-thiolate and 365 ml of N-methyl-2-pyrrolidone were added and, after 30 min at 0° C., 14.2 ml of iodomethane were added dropwise. After 2 hours at 0° C., the reaction mixture was carefully adjusted to pH 2 using concentrated aqueous hydrochloric acid. About 200 ml of water were added, and the precipitated solid was filtered off with suction, washed with water until neutral and dried under reduced pressure. This gave 50.89 g (67%) of the title compound, which was reacted further without any further purification.
Wird geladen…
