According to the analysis of related databases, 641571-11-1, the application of this compound in the production field has become more and more popular.
Electric Literature of 641571-11-1, 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 641571-11-1 as follows.
Example 30[00103] Form A of the free base of 4-methyl-N-[3-(4-methyl-imidazol-l-yl)-5- trifluoromethyl-phenyl] -3 -(4-pyridin-3 -yl-pyrimidin-2-ylamino)-benzamide is made according to the following scheme:Eq.)10 EPO [00104] 14.5 g (60.0 mmol) of B6 and 20.8 g (64.8 mmol) of B5 are dissolved in 120 niL tetrahydrofuran absolute at room temperature under inert and water-free conditions. The suspension is cooled to IT 0-5C and 101.0 g (180 mmol) of potassium tert-butoxide solution 20% in tetrahydrofuran were added within 1 hour, maintaining the internal temperature at 0-5C. The reaction mixture is heated gradually to IT 5O0C within 1 hour and then stirred at this temperature for another 1 hour. The reaction mixture (yellow suspension) is quenched at IT 50C by the addition of 50 mL of water. Stirring is stopped, and the two phase system is let to separate. The aqueous (lower) phase is removed. Seeding crystals (0.2 g) of form A are added to the remaining organic phase, and the thin suspension is stirred for 1 hour at 500C during which time crystallization is initiated. Approximately 1.0 mL of acetic acid is added to the organic phase until a pH of ~10 is reached. Solvent (260 mL) is distilled off at 80-1000C (external temperature) under normal pressure, and simultaneously 260 mL ethanol 94% is added keeping the volume constant, i.e., solvent exchange from tetrahydrofuran to ethanol. The suspension is cooled to IT 0-50C within 1 hour, and agitation is continued for another 1 hour. Form A of the free base of 4-methyl-N-[3-(4-methyl-imidazol-l-yl)-5- trifluoromethyl-phenyl] -3 -(4-pyridin-3 -yl-pyrimidin-2-ylamino)-benzamide (crystalline solid) is collected by filtration and washed with 150 mL of cold ethanol 94%. The product is then dried at 500C in vacuo.
According to the analysis of related databases, 641571-11-1, the application of this compound in the production field has become more and more popular.