【正文】
d medicine intermediate. The research content of the subject is the synthesis of 2,6difluorine4amino pyrimidine. Potassium fluoride and sulfolane go through vacuum distillation firstly, and 2,4,6trichloro pyrimidine will be added later for synthetizing of trifluoropyrimidine. And then sodium amide is added into trifluoropyrimidine to synthetize 2,6difluorine4aminopyrimidine. Inspected by the molar ratio, reaction time, temperature, pressure and other factors, productive rate of 2,6difluorine4amino pyrimidine can increase. The control variate method is used to control norm of reaction and reaction conditions and reference literatures and analysis of experimental variables. In order to improve the yield of product, each step reaction is carried on certain optimization to obtain a good result. Studies have shown that the molar ratio of potassium fluoride and 2,4,6trichloropyrimidine is :1 at 160oC, trichloropyrimidine yield is up to 68%. Trichloropyrimidine reacts with Sodium amide at 65oC, the highest yield of 2,6difluorine4aminopyrimidine is 78%. The final product and intermediate products were determined by HNMR, mass spectrometry analysis. Keywords:2,6difluorine4aminopyrimidine。通過(guò) 考察 摩爾配比,反應(yīng)時(shí)間,溫度,壓力等因素, 以 提高 2,6二氟 4氨基嘧啶的產(chǎn)率。嘧啶類(lèi)化合物具有重要的生物活性,廣泛應(yīng)用于殺蟲(chóng)劑、除草劑、殺菌劑和醫(yī)藥中間體而倍受人們關(guān)注。 本課題研究的內(nèi)容是 2,6二氟 4氨基嘧啶的合成。 為了提高產(chǎn)品的產(chǎn)率, 通過(guò)對(duì)文獻(xiàn)的參考 和 實(shí)驗(yàn)變量 的 分析 , 控制變量法控制反應(yīng)量和反應(yīng)條件, 對(duì)各步反應(yīng)進(jìn)行一定的優(yōu)化,獲得了很好的結(jié)果。 2,4,6trichloropyrimidine。 1. 緒論 ................................................................ 1 嘧啶類(lèi)化合物的意義 .............................................................................................. 1 2氨基嘧啶主要的應(yīng)用 ........................................................................................... 1 有機(jī)合成方面 ................................................................................................ 1 醫(yī)藥方面 ........................................................................................................ 1 鹵代嘧啶的合成方法 .............................................................................................. 2 2氨基 4,6二氯嘧啶的合成 ......................................................................... 2 2氨基 4,6二氯嘧啶的合成 ......................................................................... 2 5溴嘧啶衍生物的合成 [12~15] ........................................................................ 2 4,6二氯嘧啶的合成 ...................................................................................... 2 4取代 2氨基嘧啶衍生物的合成 [7] ............................................................. 3 N’(4,6二取代嘧啶 2基 )氧化煙酰硫脲的合成與生物活性測(cè)定 [5] .......... 3 論文研究方案 .......................................................................................................... 3 ............................................................................................................................ 5 試劑及儀器 ............................................................................................................. 5 實(shí)驗(yàn)試劑(見(jiàn)表 1) ..................................................................................... 5 實(shí)驗(yàn)儀器(見(jiàn)表 2) ..................................................................................... 5 實(shí)驗(yàn)原理 .................................................................................................................. 5 典型合成步驟 .......................................................................................................... 6 三氟嘧啶的合成 [11] ........................................................................................ 6 2氨基 4,6二 氟 嘧啶的合成 ......................................................................... 6 產(chǎn)物測(cè)定 ........................................................................................................ 6 ........................................................................................................................ 7 三氟嘧啶的合成 ..................................................................................................... 7 反應(yīng)配比對(duì)三氟嘧啶產(chǎn)率的影響 ................................................................ 7 溫度對(duì)三氟嘧啶產(chǎn)率的影響 ........................................................