7752-72-9
7752-72-9 結(jié)構(gòu)式
基本信息
5-氯-6-甲基嘧啶-4(1H)-酮
5-氯-6-甲基嘧啶-4(3H)-酮
5-氯-6-甲基-4(3H)-嘧啶酮
4-羥基-5-氯-6-甲基嘧啶 100MG
4-Chloro-6-methyl-pyrimidin-5-ol
5-Chloro-6-methyl-1H-pyrimidin-4-one
5-CHLORO-6-METHYLPYRIMIDIN-4(1H)-ONE
5-Chloro-6-MethylpyriMidin-4(3H)-one
5-Chloro-6-hydroxy-4-methylpyrimidine
4(3H)-Pyrimidinone, 5-chloro-6-methyl-
4(1H)-Pyrimidinone, 5-chloro-6-methyl- (9CI)
物理化學(xué)性質(zhì)
制備方法
3473-63-0
609-15-4
7752-72-9
以醋酸甲脒和2-氯乙酰乙酸乙酯為原料合成5-氯-6-甲基嘧啶-4(1H)-酮的一般步驟如下：將4-羥基-5-氯-6-甲基嘧啶（8.80g，0.16mol）的甲醇溶液緩慢加入到含有11.30g（0.11mol）醋酸甲脒的50mL甲醇溶液中，反應(yīng)在室溫下攪拌進(jìn)行。加入完畢后，繼續(xù)在室溫下攪拌混合物2小時。隨后，加入11.17g（0.068mol）2-氯-3-氧代丁酸乙酯，室溫下繼續(xù)攪拌反應(yīng)5-7小時。反應(yīng)進(jìn)程通過薄層色譜（TLC）監(jiān)測。反應(yīng)完成后，將反應(yīng)混合物減壓濃縮，用鹽酸（HCl）調(diào)節(jié)pH至5-6，過濾得到橙黃色固體。水相用乙酸乙酯（3×50mL）萃取，合并有機(jī)相，用無水硫酸鎂干燥，過濾后減壓濃縮。將殘余物溶于50mL乙酸乙酯中，靜置過夜，得到6.48g橙黃色固體產(chǎn)物，產(chǎn)率為66%，熔點為181~184°C。
參考文獻(xiàn)：
[1] Patent: EP2913325, 2015, A1. Location in patent: Paragraph 0451; 0452
[2] Patent: CN105348298, 2016, A. Location in patent: Paragraph 0418; 0419; 0420
[3] Patent: CN105732585, 2016, A. Location in patent: Paragraph 0368; 0369; 0370
[4] Patent: CN105777717, 2016, A. Location in patent: Paragraph 0356; 0357; 0358; 0359
[5] Patent: CN104292169, 2018, B. Location in patent: Paragraph 0457; 0458; 0459