摘要
以30%(质量分数)的双氧水为氧化剂,钨酸钠与含O的双齿有机配体(草酸)形成的络合物为催化剂,在无有机溶剂、无相转移剂的条件下,研究了4,6-二甲氧基-2-甲巯基嘧啶(d)催化氧化合成4,6-二甲氧基-2-甲磺酰基嘧啶(e)的反应。实验表明,用草酸为配体,当原料DMCP(d)用量为100mmol时,较佳反应条件为钨酸钠∶草酸∶4,6-二甲氧基-2-甲巯基嘧啶的物质的量比为3.0∶5.0∶100,30%(质量分数)双氧水的体积为35mL,在65～70℃下反应6h,可制得的4,6-二甲氧基-2-甲磺酰基嘧啶。并通过HPLC,IR和1H-NMR对目标产品进行了分析。以4,6-二甲氧基-2-甲巯基嘧啶计,氧化收率>88%,目标产品HPLC纯度大于99%。
The oxidation of DMCP to DMSP by 30 % aqueous hydrogen peroxide catalyzed by coordination compound system formed between sodium tungstate and didentate ligands containing O atom such as oxalic acid without phase transfer agent and organic solvent was investigated. The better reaction conditions were obtained by experiments, when the raw material dosage of DMCP（d） was 100 mil-molar, the optimal conditions of reaction were that reactant molar ratio of sodium tungstate dehydrate, oxalic acid, DMCP, 30 % aqueous hydrogen peroxide was found to be 3.0-5.0, 100, the volume of 30% aqueous hydrogen peroxide was 35 milliliter, the process reaction time was 6 h, and process temperature was 65-70 ℃. The destination product was identified with HPLC,IR and ^1H-NMR. Its oxidation yield was over 88 % by DMCP and over 99 % purity product was attained.
出处
《中国钨业》
CAS
北大核心
2008年第4期38-41,共4页
China Tungsten Industry
基金
江西省教育厅科技资助项目(GJJ08440)
