403-01-0

基本信息
甲基 3-氟-4-羥基苯酸鹽
甲基 3-氟-4-羥基苯甲酸酯
Fluoro-4-hydroxybenzoate
METHYL 3-FLUORO-4-HYDROXYBENZOATE
3-FLUORO-4-HYDROXY-BENZOIC ACID METHYL ESTER
Benzoic acid, 3-fluoro-4-hydroxy-, methyl ester
物理化學(xué)性質(zhì)
制備方法

67-56-1

350-29-8

403-01-0
3-氟-4-羥基苯甲酸甲酯(T10.1)的合成步驟:在圓底燒瓶中加入3-氟-4-羥基苯甲酸(5.03g,32.22mmol,可商購自Sigma-Aldrich,St.Louis,MO,USA)、甲醇(50.0mL)和冷硫酸(2.0mL)。將反應(yīng)混合物加熱至80℃,并通過薄層色譜(TLC)監(jiān)測反應(yīng)進程。反應(yīng)20.5小時后,減壓蒸餾除去溶劑。將殘余物用乙醚稀釋,有機相依次用飽和碳酸氫鈉水溶液洗滌兩次、鹽水洗滌一次,隨后用無水硫酸鈉干燥。過濾后,減壓蒸發(fā)除去有機溶劑,得到白色固體狀產(chǎn)物T10.1(4.79g,收率87%)。產(chǎn)物經(jīng)1H NMR(400MHz,CDCl3)表征:δ 7.81(2H,m),7.06(1H,t,J = 8.4Hz),5.62(1H,d,J = 4.3Hz),3.91(3H,s)。
參考文獻:
[1] Patent: WO2010/45258, 2010, A2. Location in patent: Page/Page column 155
[2] Patent: WO2009/111056, 2009, A1. Location in patent: Page/Page column 227-228
[3] Patent: WO2008/87529, 2008, A1. Location in patent: Page/Page column 42; 43; 119-120
[4] Patent: WO2010/9290, 2010, A1. Location in patent: Page/Page column 58
[5] Patent: US2007/191603, 2007, A1. Location in patent: Page/Page column 35