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. 830346-47-9, name is 1-(2-Fluoro-6-(trifluoromethyl)benzyl)-6-methylpyrimidine-2,4(1H,3H)-dione, molecular formula is C13H10F4N2O2, 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. Quality Control of 1-(2-Fluoro-6-(trifluoromethyl)benzyl)-6-methylpyrimidine-2,4(1H,3H)-dione
Step 1D: Preparation of 5-bromo-1-[2-fluoro-6-(trifluoromethyl)benzyl]-6- methylpyrimidine-2,4 (1H,3H)-dione 1-1; Bromine (16.5 mL, 0.32 mmol) was added to 1-[2-fluoro-6- (trifluoromethyl)benzyl]-6-methylpyrimidine-2,4(IH,3H)-dione 1c (48.5 g, 0.16 mol) in 145 mL of acetic acid. The resulting mixture became clear then formed precipitate within an hour. After 2 hours stirring, the yellow solid was filtered and washed with cold EtOAc to an almost white solid. The filtrate was washed with sat. NaHC03 and dried over Na2S04. Evaporation gave a yellow solid which was washed with EtOAC to give a light yellow solid. The two solids were combined to give 59.4 g of 1-1 (0.156 mol) total. 1H NMR (CDC13) No. 2.4 (3H, s), 5.48 (2H, s), 7.25 – 7.58 (3H, m), 8.61 (1H, s) ; MS (CI) m/z 380.9 (MH+).
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Reference:
Patent; NEUROCRINE BIOSCIENCES, INC.; WO2005/113516; (2005); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia