Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 874-14-6, name is 1,3-Dimethyluracil. A new synthetic method of this compound is introduced below., Computed Properties of C6H8N2O2
10405] A solution of 1H-pyrazol-5-amine and 1,3-dimeth- ylpyrimidine-2,4(1H,3H)-dione (1.05 equiv.) were charged to a round bottom flask outfitted with a mechanical stirrer,steam pot, a reflux condenser, a J-Kem temperature probe and an N2 adaptor for positive N2 pressure control. Under mechanical stirring the solids were suspended with 4 vol. (4 mL/g) of absolute EtOR under a nitrogen atmosphere, then charged with 2.1 equivalents of NaOEt (21 wt percent solution in EtOR), and followed by line-rinse with 1 vol. (1 mL/g) of absolute EtOR. The slurry was warmed to about 75° Celsius and stirred at gentle reflux until less than 1 .5 area percent of 1H-pyrazol-5-amine was observed by TRK1PM1 HPLC tofollow the progression of the reaction using 20 tL of slurry diluted in 4 mE deionized water and 5 tE injection at 220 mm10406] After 1 additional hour, the mixture was charged with 2.5 vol. (2.5 mE/g) of heptane and then refluxed at 70° Celsius for 1 hout The slurry was then cooled to room temperature overnight. The solid was collected by filtrationa tabletop funnel and polypropylene filter cloth. The reactor was rinsed and charged atop the filter cake with 4 vol. (4 mE/g) of heptane with the cake pulled and the solids being transferred to tared drying trays and oven-dried at 45° Celsius under high vacuum until their weight was constant. Pale yellow solid sodium pyrazolo[1 ,5-a] -pyrimidin-5-olate was obtained in 93-96percent yield (corrected) and larger than 99.5 area percent observed by HPEC (1 mgmE dilution in deionized water, TRK1PM1 at 220 nm).
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Reference:
Patent; Loxo Oncology, Inc.; Cox, Michael; Nanda, Nisha; (65 pag.)US2017/281632; (2017); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia