以乙酰乙酸乙酯和尿素为原料,用对甲苯磺酸作催化剂合成6-甲基尿嘧啶,探讨了不同相转移催化剂、带水剂、相转移催化剂用量及脱水缩合时间等因素对反应产物产率的影响。得出最佳工艺条件为:19.8mL乙酰乙酸乙酯、10g尿素,对甲苯磺酸1.2g,150mL石油醚作带水剂,0.3g聚乙二醇200作相转移催化剂,回流脱水缩合8h,产率可达78%。
6-meyhyl uracil was synthesized from ethyl acetoacetate and urea with p-toluenesulfonic acid as cata-lyst. The effects of phase transfer catalysts, water-carrying agents, amount of phase transfer catalyst and reaction time on yield of 6-meyhyl uracil were studied. The optimum conditions were as follows:fixed ratio of raw materials n(urea) ∶ n(ethylacetoacetate) =0. 167mol ∶0. 157mol =1. 06 ∶1,the amount of p-toluenesulfonic acid 1. 2g;150 mL petroleum ether as water-carrying agent;0. 3 g polyethylene glycol 200 as phase transfer catalyst;reaction time 8h;and reaction temperature 72℃,the yield of 6-meyhyl uracil was 78%.
参考文献
[1] | Starrett J J E;Mansuri M M;Martin J C et al.{?}Production of 2′,3′-Dideoxy-2′,3′-Didehydro-nucleosides[P].EP,334 368,1989. |
[2] | 张新迎,王洋洋,冯东,范学森.5-取代嘧啶核苷类似物的设计、合成及生物活性研究进展[J].有机化学,2010(06):797-808. |
[3] | D' Souza R;Kiss J .Process for the preparation of 5′-deoxy-5-fluoro uridine and intermediates in this process[P].EP,21231,1981. |
[4] | 张泉,黄明智,闵忠诚,谌伟民.具除草活性的脲嘧啶类化合物的研究进展[J].农药,2006(02):73-77. |
[5] | 李公春,朱有全,杨风岭,杨华铮.苄基脲嘧啶类化合物的合成及其除草活性[J].合成化学,2011(01):111-114. |
[6] | 李公春,鞠志宇,吴长增,杨风岭.新型脲嘧啶类化合物的合成及其除草活性[J].贵州农业科学,2013(07):108-110. |
[7] | 李公春,吴长增,朱有全,杨风岭,杨华铮.6-三氟甲基嘧啶-2,4(1H,3H)-二酮类化合物的合成及其除草活性[J].合成化学,2013(02):231-233,244. |
[8] | 李东光;翟怀风 .2-氯-4-二甲胺基-6-甲基嘧啶的合成[J].河北化工,1998,31(2):1-3. |
[9] | 蒋忠良,汪正发,马东旭,周煜磊.6-甲基尿嘧啶的合成研究[J].同济大学学报(自然科学版),2003(02):250-252. |
[10] | 丁欣宇;李建华.相转移催化合成6-甲基尿嘧啶[J].化学世界,2004(8):489-492. |
[11] | 吴建一,冯德明.十六烷基三甲基溴化铵催化合成6-甲基尿嘧啶的研究[J].化学与粘合,2001(04):153-155. |
[12] | 耿静漪,姜文清,贾定先.6-甲基尿嘧啶的绿色合成[J].实验室科学,2013(01):8-10. |
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