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Citation: WANG Haitao, WANG Hongyan, YANG Liangru, MAO Pu, QU Lingbo. Process Optimization of 4-Hydroxyl-2-(methylsulfanyl)-pyrimidine-5-carboxylic Acid Ethyl Ester Synthesis[J]. Chinese Journal of Applied Chemistry, ;2015, 32(4): 412-415. doi: 10.11944/j.issn.1000-0518.2015.04.140294 shu

Process Optimization of 4-Hydroxyl-2-(methylsulfanyl)-pyrimidine-5-carboxylic Acid Ethyl Ester Synthesis

1.
School of Chemistry and Chemical Engineering, He ban University of Technology, Zhengzhou 450000, China

Corresponding author: YANG Liangru,
Received Date: 25 August 2014
Available Online: 17 December 2014
Fund Project: 国家自然科学基金资助项目(21172055) (21172055)

4-Hydroxyl-2-(methylsulfanyl)-pyrimidine-5-carboxylic acid ethyl ester was synthesized from S-methylisothiourea hemisulfate salt and diethyl ethoxymethylenemalonate in ethanol. The feed ratio,reaction temperature,reaction time and other factors were optimized to improve the yield. The 81.1% yield of white solid product is obtained when the sodium hydroxide solution is dropwisely added into the reaction mixture in a molar ration of n(C₂H₆N₂S·1/2H₂SO₄):n(C₁₀H₁₆O₅):n(NaOH)=1.2:1:1.8 under stirring at room temperature for 6 h then with acid treatment. Its structure was characterized by melting point,¹H NMR,ESIMS and FT-IR.
- hydroxyl-(methylsulfanyl)-pyrimidine-carboxylic acid ethyl ester,
- optimization,
- pyrimidine derivatives
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