915107-31-2

基本信息
6-Chloro-5-methoxy-nicotinic acid methyl ester
Methyl 6-chloro-5-Methoxypyridine-3-carboxylate
3-Pyridinecarboxylic acid, 6-chloro-5-methoxy-, methyl ester
Methyl 6-chloro-5-methoxypyridine-3-carboxylate, 2-Chloro-3-methoxy-5-(methoxycarbonyl)pyridine
物理化學(xué)性質(zhì)
制備方法

915107-30-1

74-88-4

915107-31-2
以6-氯-5-羥基煙酸甲酯(1.8 g,9.6 mmol)、碘甲烷(2M乙醚溶液,5.8 mL,11.6 mmol)和碳酸鉀(2.0 g,14.5 mmol)為原料,在丙酮(190 mL)中回流反應(yīng)6小時。反應(yīng)完成后,使用旋轉(zhuǎn)蒸發(fā)儀濃縮反應(yīng)混合物,隨后加入水(100 mL)進行稀釋。通過過濾收集生成的白色沉淀,并用額外的水洗滌,得到目標產(chǎn)物6-氯-5-甲氧基煙酸甲酯,為白色固體(1.33 g,收率68%),熔點為83-85℃。產(chǎn)物結(jié)構(gòu)通過1H NMR(400 MHz,CDCl3)δ 8.60(d,1H)、7.77(d,1H)、3.98(s,3H)、3.96(s,3H)和GC-MS(計算值:C8H8ClNO3 [M]+ 201,實測值:201)進行確認。
參考文獻:
[1] Patent: US2009/131468, 2009, A1. Location in patent: Page/Page column 66
[2] Patent: WO2009/64251, 2009, A1. Location in patent: Page/Page column 140
[3] Patent: US2008/108667, 2008, A1. Location in patent: Page/Page column 10
[4] Patent: US2016/376283, 2016, A1. Location in patent: Paragraph 0493; 0495
[5] Patent: WO2011/48525, 2011, A1. Location in patent: Page/Page column 44