102625-64-9 , The common heterocyclic compound, 102625-64-9, name is 5-(Difluoromethoxy)-2-(((3,4-dimethoxypyridin-2-yl)methyl)thio)-1H-benzo[d]imidazole, molecular formula is C16H15F2N3O3S, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
At room temperature, 10.0 G of 5-DIFLUOROMETHOXY-2- [ (3, 4-DIMETHOXY-2-PYRIDINYL) METHYLTHIO]-1H- benzimidazole and 1.05 G of (+) -L-tartaric acid bis- (N-pyrrolidinamide) (0.15 eq. ) are suspended in 72 ML of methyl isobutyl ketone. The suspension is heated at 40-45C and 12 ml of MIBK are distilled off for azeotropic removal of water present in the mixture. At this temperature, 0.53 G of zirconium (IV) ISOPROPOXIDE-ISOPROPANOL (0.05 eq. ) is added and the mixture is stirred for 1 hour. After cooling to 30C, 0.16 mi of N-ETHYIDIISOPROPYLAMINE is added. 5.5 g of cumene hydroperoxide (80% in cumene) are then slowly metered in. Stirring is continued at 30C until the exothermic oxidation process has ended (20 hours, monitored by TLC or HPLC). HPLC of the reaction shows 82% of title compound in an optical purity of > 95%.
The synthetic route of 102625-64-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ALTANA PHARMA AG; WO2004/52881; (2004); A2;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem