Application of 313339-35-4, 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. 313339-35-4, name is 4,6-Dichloro-2-(methylthio)pyrimidine-5-carboxylic acid, molecular formula is C6H4Cl2N2O2S, 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.
Reference Example 70 Production of ethyl 4,6-dichloro-2-(methylsulfanyl)pyrimidine-5-carboxylate To a solution of the compound of Reference Example 69 (4.02 g, 18 mmol), amidosulfuric acid (3.50 g, 36 mmol), tert-butanol (72 mL), THF (72 mL) and water (36 mL) was added a solution of sodium chlorite (2.03 g, 18 mmol) in water (36 mL) at -10C, and the mixture was stirred for 10 min. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed successively with 1% aqueous sodium thiosulfate solution and brine, dried over magnesium sulfate, and concentrated under reduced pressure to give 4,6-dichloro-2-(methylsulfanyl)pyrimidine-5-carboxylic acid as a crude product. To a solution of this crude product in THF (50 mL) were added oxalyl chloride (2.36 mL, 27 mmol) and DMF (1 drop), and the mixture was stirred at room temperature for 1 hr. Water was added thereto, and the mixture was extracted twice with ethyl acetate. The extract was washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure. To the residue were added ethanol (50 mL) and triethylamine (3.76 mL, 27 mmol), and the mixture was stirred at room temperature for 2 hr. The reaction mixture was concentrated under reduced pressure, aqueous sodium hydrogen carbonate solution was added thereto, and the mixture was extracted twice with ethyl acetate. The extract was washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluate, hexane:ethyl acetate=99:1?90:10) to give the title compound (3.28 g, 68%) as a pale-yellow oil. 1H NMR (300 MHz, CDCl3) delta:1.41 (3 H, t, J = 7.2 Hz), 2.59 (3 H, s), 4.45 (2 H, q, J = 7.1 Hz).
While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 313339-35-4, 4,6-Dichloro-2-(methylthio)pyrimidine-5-carboxylic acid.
Reference:
Patent; Takeda Pharmaceutical Company Limited; EP2471793; (2012); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia