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 6228-73-5 as follows. Quality Control of Cyclopropanecarboxamide
Cyclopropanecarboxamide (22.5 mg, 0.26 mmol) was combined with Int3 (30 mg, 0.088 mmol). Dimethylacetamide (DMA, 0.6 mL) was added to the vessel, followed by the addition of tris (diphenylmethyleneacetone) dicum (0) (Pd2dba3, 8.1 mg, 0.0088 mmol)4,5-bis (diphenylphosphino) -9,9-dimethyl(Xantphos, 10 mg, 0.018 mmol) and cesium carbonate (115 mg, 0.35 mmol). The vessel was then evacuated and backfilled three times with nitrogen and heated to 145 & lt; 0 & gt; C for 1 hour.The reaction was cooled to room temperature and then diluted with ethyl acetate (EtOAc, ca. 250 mL). The solution was washed twice with water, dried over sodium sulfate (Na2SO4), filtered, concentrated and purified using preparative HPLC. The product in the form of TFA salt was collected and then dissolved in about 15 mL of water, to which about 100 mL of saturated sodium bicarbonate (NaHCO3, an aqueous solution) was added and stirred for 10 minutes. The product of (x3) was extracted from the slurry using dichloromethane (DCM), dried over sodium sulfate, filtered, concentrated and collected to give 16.3 mg of 1 (48% yield).
According to the analysis of related databases, 6228-73-5, the application of this compound in the production field has become more and more popular.
Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; MOSLIN,, RYAN M.; WEINSTEIN,, DAVID S.; WROBLESKI,, STEPHEN T.; ZHANG,, YANLEI; TOKARSKI,, JOHN S.; MERTZMAN,, MICHAEL E.; LIU,, CHUNJIAN; (124 pag.)TWI582077; (2017); B;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics