Reference of 959236-97-6 , The common heterocyclic compound, 959236-97-6, name is 4-Bromo-2-(methylthio)pyrimidine, molecular formula is C5H5BrN2S, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
To stirred 30% H202 (6g, 29.4 mmol, 1 eq) was added ammonium molybdate tetrahydrate (1.09g, 0.88mmol, 0.03eq) at 0C portion wise then stirred for 20min., and then a solution of 4-bromo-2-(methylthio)pyrimidine (6g, 29.41mmol, leq) slowly added at 0C then allowed to RT for 3h. Monitored by TLC, the reaction mixture was concentrated to crude residue, which was diluted with cold water then extracted with DCM (3X100mL). The combined organic layer was washed with 5% H2SC>4 solution and water then dried over Na2SC>4 and concentrated to crude compound. The crude compound was purified by column chromatography (silica gel, 100-200 mesh) using 0-40% EtOAc in pet ether as eluent to afford 4-bromo-2- (methylsulfonyl)pyrimidine (6g, 86%) as off-white solid. LCMS: [M+H]+ 238.84.
The synthetic route of 959236-97-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ONTARIO INSTITUTE FOR CANCER RESEARCH (OICR); AL-AWAR, Rima; ZEPEDA-VELAZQUEZ, Carlos Armando; PODA, Gennady; ISAAC, Methvin; UEHLING, David; WILSON, Brian; JOSEPH, Babu; LIU, Yong; SUBRAMANIAN, Pandiaraju; MAMAI, Ahmed; PRAKESCH, Michael; STILLE, Julia Kathleen; (1053 pag.)WO2017/147700; (2017); A1;,
Pyrimidine | C4H4N2 – PubChem,
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