Related Products of 52189-63-6, These common heterocyclic compound, 52189-63-6, name is 1-Fluoro-3,5-dimethoxybenzene, 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.
28.22 g of 3,5-dimethoxy-5-fluorobenzene was weighed into a 1,000 mE round bottom flask fitted with a stir bar, reflux condenser, nitrogen inlet, and cap. A nitrogen atmosphere was established and maintained throughout the reaction. 200 mE of anhydrous CC14 was added, followed by 32.61 g of N-bromosuccinimide (NI3S). The remaining NI3S powder residue was washed into the flask with 100 mE of CC14. The reaction mixture was stirred at reflux under N, for 4 h, during which time the suspended yellow solids changed color to white. At completion, the precipitated succinimide solids were filtered off and washed thoroughly with 200 mE heptane. The CC14 was removed from the filtrate by rotary evaporation at 50 C. More succinimide precipitated from the heptane solution and was removed by filtration while the solution was still warm. The remaining heptane was removed in vacuo to obtain a clear, amber oil (40.67 g), which solidified on standing. Purification of the crude material was accomplished by distillation. The condenser was kept at 50 C. to prevent the product from solidi1zing before reaching the collection flask. After a small impurity fraction was collected at 78 C./8 torr, the product distilled at 123-125 C./8 ton. The clear pale yellow liquid solidified to an off-white solid on standing (37.88
The synthetic route of 52189-63-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; HINMAN, Andrew W.; Davis, Dana; Kheifets, Viktoria; US2014/256830; (2014); A1;,
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