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 59989-18-3 as follows., 59989-18-3
under protection of argon, the cuprous iodide (0.02 mmol, 3.8 mg), four-triphenylphosphine palladium (0.02 mmol, 23 mg) and 1 – octane, 5 – ethynyl uracil (0.4 mmol, 99.6 mg) are added to the 4, 4 – di (3, 4, 5 – c (dodecyl) benzyl alkyne base) – 2, 6 – diiodosalicylic -8 – (3, 4, 5 – c (dodecyl) phenyl) beryllium two pyrrole in (0.2 mmol, 480 mg). For syringe triethylamine (5 ml) is injected into the mixture and, in the 70 C reaction in oil bath for four hours. Thin layer chromatographic detection, to be the reaction is complete, the reaction also adding 20 ml water quenching reaction. Ethyl ether (3 ¡Á 40 ml) extraction product, organic phase water (3 ¡Á 40 ml) washing three times. Anhydrous magnesium sulfate drying, pressure reducing and steaming and in addition to the solvent. The crude product column chromatographic separation and purification, showering liquid to dichloromethane: ethyl acetate=50:1, volume ratio. The product methanol recrystallization is purple solid, 179.5 mg, yield is 68%.
The chemical industry reduces the impact on the environment during synthesis 59989-18-3, I believe this compound will play a more active role in future production and life.
Reference:
Patent; Tianjin University; Chen Zhijian; Liu Ping; (17 pag.)CN107056829; (2017); A;,
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