合成化学
閤成化學
합성화학
CHINESE JOURNAL OF SYNTHETIC CHEMISTRY
2010年
1期
118-120
,共3页
2-硫脲嘧啶%硫脲%一锅法%合成
2-硫脲嘧啶%硫脲%一鍋法%閤成
2-류뇨밀정%류뇨%일과법%합성
2-thiouracil%one-pot method%thiourea%synthesis
采用一锅法合成了2-硫脲嘧啶,最佳反应条件为:硫脲33 mmol,n(乙酸乙酯):n(甲酸乙酯):n(甲醇钠):n(硫脲)=2.5:2.0:1.5:1.0;乙酸乙酯与甲醇钠在甲苯(35 mL)中于80 ℃反应3 h;冷却后滴加甲酸乙酯,于25 ℃充分搅拌8 h后加入硫脲的乙醇(10 mL)溶液,回流反应3 h,收率54.7%.
採用一鍋法閤成瞭2-硫脲嘧啶,最佳反應條件為:硫脲33 mmol,n(乙痠乙酯):n(甲痠乙酯):n(甲醇鈉):n(硫脲)=2.5:2.0:1.5:1.0;乙痠乙酯與甲醇鈉在甲苯(35 mL)中于80 ℃反應3 h;冷卻後滴加甲痠乙酯,于25 ℃充分攪拌8 h後加入硫脲的乙醇(10 mL)溶液,迴流反應3 h,收率54.7%.
채용일과법합성료2-류뇨밀정,최가반응조건위:류뇨33 mmol,n(을산을지):n(갑산을지):n(갑순납):n(류뇨)=2.5:2.0:1.5:1.0;을산을지여갑순납재갑분(35 mL)중우80 ℃반응3 h;냉각후적가갑산을지,우25 ℃충분교반8 h후가입류뇨적을순(10 mL)용액,회류반응3 h,수솔54.7%.
2-Thiouracil was synthesized by one-pot method.The yield could reach 54.7% under the optimum reaction conditions.Thiourea was 33 mmol.n(ethyl acetate):n(sodium methoxide):n(ethyl formate):n(thiourea) was 2.5:2.0:1.5:1.0.Ethyl acetate reacted with sodium methoxide in 35 mL toluene at 80 ℃ for 3 h,then ethyl formate was added dropwise at 25 ℃,and thiourea in 10 mL alcohol was added after stirring at 25 ℃ for 8 h,followed by refluxing for 3 h.
