54346-19-9

基本信息
pyrazolo[1,5-a][1,3,5]triazine
4-chloro-2-(Methylthio)pyrazolo[1
4-CHLORO-2-METHYLTHIOPYRAZOLO[1,5-A]1,3,5-TRIAZINE
Pyrazolo[1,5-a]-1,3,5-triazine, 4-chloro-2-(methylthio)-
4-Chloro-2-methylsulfanyl-pyrazolo[1,5-a][1,3,5]triazine
4-chloro-2-(methylthio)-1,2-dihydropyrazolo[1,5-a][1,3,5]triazine
物理化學(xué)性質(zhì)
制備方法
![2 - (甲硫基)吡唑并[1,5-A][1,3,5]三嗪-4 - 醇](/CAS/GIF/54346-18-8.gif)
54346-18-8
![4-氯-2-(甲硫基)吡唑并[1,5-A][1,3,5]三嗪](/CAS/GIF/54346-19-9.gif)
54346-19-9
以2-(甲硫基)吡唑并[1,5-α][1,3,5]三嗪-4(3H)-酮為原料合成4-氯-2-(甲硫基)吡唑并[1,5-a][1,3,5]三嗪的一般步驟如下:在室溫下,向攪拌中的2-(甲硫基)吡唑并[1,5-α][1,3,5]三嗪-4(3H)-酮(2.0g,11mmol)和三氯氧磷(20mL)的懸浮液中加入N,N-二乙基苯胺(0.7mL)。將反應(yīng)混合物加熱至回流溫度。反應(yīng)1.5小時后,將混合物冷卻至室溫并減壓濃縮。將殘余物溶解于甲苯中,有機(jī)層用鹽水洗滌后再次減壓濃縮,得到4-氯-2-(甲硫基)吡唑并[1,5-a][1,3,5]三嗪(2.0g,收率91%)。TLC Rf = 0.57(乙酸乙酯/己烷,1/3);1H NMR(300MHz,CDCl3)δ 8.15(d,J = 2.2Hz,1H),6.50(d,J = 2.2Hz,1H),2.60(s,3H)。
參考文獻(xiàn):
[1] Bioorganic and Medicinal Chemistry, 2011, vol. 19, # 20, p. 5955 - 5966
[2] Patent: US2007/78136, 2007, A1. Location in patent: Page/Page column 50
[3] Patent: WO2011/31979, 2011, A1. Location in patent: Page/Page column 147
[4] Patent: US9303033, 2016, B2. Location in patent: Page/Page column 285; 286
[5] Patent: JP5802676, 2015, B2. Location in patent: Paragraph 0552