In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 458-52-6 as follows. Recommanded Product: 2-Fluoro-4-methoxyaniline
A mixture of (+-)-4-[trans-3-(tert-butyl-dimethyl-silanyloxy)-cyclopentyl-amino]-2-methylsulfanyl-pyrimidine-5-carbaldehyde (171 mg, 0.46 mmol) (from Example 13a supra), p-toluenesulfonic acid mono-hydrate (10 mg) (Aldrich) and 2-fluoro-4-methoxyaniline (79 mg, 0.56 mmol) (from Example 14a supra) in benzene (30 ML) was refluxed in a Dean-Stark apparatus for 8 hours.The mixture was then cooled and partitioned between ethyl acetate and saturated aqueous potassium carbonate.The organic layer was collected, dried over sodium sulfate, filtered and concentrated.The residue was dissolved in anhydrous tetrahydrofuran (50 ML) and to this solution was added in small portions lithium aluminum hydride (53 mg, 1.40 mmol) (Aldrich) at 0¡ã C. The slurry was allowed to slowly warm up to room temperature and after overnight stirring was poured slowly into a vigorously stirred mixture of ethyl acetate and saturated aqueous potassium sodium tartrate solution.The organic layer was collected, dried over sodium sulfate, filtered and concentrated to a residue that upon purification by silica gel column chromatography with a 0-60percent ethyl acetate in hexanes gradient gave (+-)-[3-trans-(tert-butyl-dimethyl-silanyloxy)-cyclopentyl]-{5-[(2-fluoro-4-methoxy-phenylamino)-methyl]-2-methylsulfanyl-pyrimidin-4-yl}-amine as a colorless viscous oil. (Yield 187 mg, 83percent). HRMS m/z calculated for C24H37FN4O2SSi [M+H]+: 493.2464. Found: 493.2472.
According to the analysis of related databases, 458-52-6, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Chen, Yi; Dermatakis, Apostolos; Liu, Jin-Jun; Luk, Kin-Chun; Michoud, Christophe; Rossman, Pamela Loreen; US2004/204427; (2004); A1;,
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