As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 10457-14-4, name is 2,4-Bis((trimethylsilyl)oxy)pyrimidine, molecular formula is C10H20N2O2Si2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. COA of Formula: C10H20N2O2Si2
A mixture of uracil (6.00 g, 53.53 mmol) and ammonium chloride (0.3 g, 5.60 mmol) in HMDS (15 ml) was refluxed for 10 h with the exclusion of moisture until a clear solution was obtained. The excess of silylating agent was removed under vacuum. The residual clear oil of 2,4-bis(trimethylsilyloxy)pyrimidine was dissolved in 25 ml of anhydrous 1,2-dichloroethane, and ethyl bromoacetate (5.92 ml, 53.53 mmol) was added. The reaction mixture was heated at reflux for 20 h, cooled to room temperature and treated with 15 ml of iPrOH. The resulting precipitate was collected and purified by flash chromatography eluting with 1:10 EtOH/1,2-dichloroethane to give 13 (9.45 g, 92%) as white crystals, mp 118-120 C, Rf 0.42 (EtOAc); 1H NMR (400 MHz, DMSO-d6) delta ppm 1.21 (3H, t, J = 7.1 Hz, CH3), 4.15 (2H, q, J = 7.1 Hz, CH2), 4.51 (2H, s, NCH2), 5.62 (1H, d, J = 7.8 Hz, H-5), 7.62 (1H, d, J = 7.8 Hz, H-6), 11.40 (1H, br s, H-3); 13C NMR (100 MHz, DMSO-d6) delta ppm 14.0, 39.1, 39.3, 39.5, 39.7, 39.9, 48.6, 61.2, 101.1, 145.9, 151.0, 163.8, 168.2.
With the rapid development of chemical substances, we look forward to future research findings about 10457-14-4.
Reference:
Article; Babkov, Denis A.; Valuev-Elliston, Vladimir T.; Paramonova, Maria P.; Ozerov, Alexander A.; Ivanov, Alexander V.; Chizhov, Alexander O.; Khandazhinskaya, Anastasia L.; Kochetkov, Sergey N.; Balzarini, Jan; Daelemans, Dirk; Pannecouque, Christophe; Seley-Radtke, Katherine L.; Novikov, Mikhail S.; Bioorganic and Medicinal Chemistry; vol. 23; 5; (2015); p. 1069 – 1081;,
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