Related Products 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.
Method same In Example 1, 0.49 g (2.03 mmol) of 4,6-dichloro-2-(methylsulfanyl)pyrimidine-5-carboxylic acid was dissolved in 20 mL of methylene chloride solvent, 0.52 g (4.06 mmol) of oxalyl chloride was added, DMF, stirred for 5 h at room temperature and the solvent and excess oxalyl chloride removed in vacuo to give a yellow solid; this was dissolved in 20 mL of dichloromethane and then 0.37 g (2.03 mmol) of 5-[(methylamino)methyl]-1H-imidazole-4-ethylformate,0.35g (3.45mmol) of triethylamine, stirred at room temperature After the reaction was completed, it was poured into 30mL of saturated sodium bicarbonate solution, extracted with dichloromethane (20mLX2), combined organic phase, dried over anhydrous sodium sulfate, filtered After the solvent was distilled off under reduced pressure, 5-((4,6-dichloro-N-methyl-2-(methylsulfanyl)pyrimidine-5-carboxamido)methyl)-1H-imidazole-4-ethylformate was obtained, used directly in the next reaction.5-((4,6-dichloro-N-methyl-2-(methylsulfanyl)pyrimidine-5-carboxamido)methyl)-1H-imidazole-4-ethylformate was dissolved in 20 mL of acetonitrile , 0.98g (7. 10mmol) of anhydrous potassium carbonate was added and the mixture was stirred at room temperature until the reaction was completed. The solvent was distilled off under reduced pressure.This was dissolved in 20 mL of methylene chloride, washed with 30 mL of saturated brine and dried over anhydrous sodium sulfate. After filtration, the solvent was evaporated under reduced pressure and the residue was purified by column chromatography (CH2C12: CH3COCH3 = 60: 1) to give a white solid The yield is 27%.0.35g (1.71mmol) of 4-chloro-2-(methylsulfanyl)pyrimidine-5-carboxylic acid was dissolved in 20mL dichloromethane solvent, 0.37g (2.94mm0l) oxalyl chloride was added, 1 drop DMF, stirred at room temperature for 6h and then under reduced pressure Evaporation of solvent and excess oxalyl chloride gave a yellow solid;This was dissolved in 20 mL of dichloromethane and then 0.22 g (1.21 mmol) of 5-[(methylamino)methyl]-1H-imidazole-4-ethylformate and 0.21 g (2.05 mmol) of triethylamine were added and stirred at room temperature After the reaction, it was poured into 30 mL of saturated sodium bicarbonate solution and extracted with dichloromethane (20 mL × 2). The combined organic phase was dried over anhydrous sodium sulfate and filtered. The solvent was evaporated under reduced pressure to give 5-((4-chloro-N-methyl-2-(methylsulfanyl)pyrimidine-5-carboxamido)methyl)-1H-imidazole-4-ethylformate was used directly in the next reaction.A solution of ethyl 5-((4-chloro-N-methyl-2-(methylsulfanyl)pyrimidine-5-carboxamido)methyl)-1H-imidazole-4-ethylformate in 20 mL of acetonitrile was added 0.58 g 4.22 mmol) anhydrous potassium carbonate and stirred at room temperature until the reaction was completed. The solvent was distilled off under reduced pressure.The residue was dissolved in 20 mL of methylene chloride, washed with 30 mL of saturated brine and dried over anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure and the residue was purified by column chromatography (CH2C12: CH3COCH3 = 10: 1) to give a white solid The yield is 60%.
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; Beijing Normal University; The Chinese People’s Liberation Army Military Academy Of Medical Sciences Poison Pharmaceutical Institute; Zhang Zhanbin; Yu Gang; Li Yi; Xiao Guiying; Cao Yanqing; Su Ruibin; Zheng Zhibing; Zhou Xinbo; (12 pag.)CN107312012; (2017); A;,
Pyrimidine | C4H4N2 – PubChem,
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