93339-98-1

基本信息
2'-氟-6'-羥基乙酰苯
1-(2-氟-6-羥基苯基)乙酮
2'-FLUORO-6'-HYDROXYACETOPHENONE
1-(2-FLUORO-6-HYDROXYPHENYL)ETHANONE
1-(2-Fluoro-6-hydroxyphenyl)ethan-1-one
Ethanone, 1-(2-fluoro-6-hydroxyphenyl)-
1-(2-Fluoro-6-hydroxyphenyl)ethan-1-one, 2-Acetyl-3-fluorophenol
物理化學性質(zhì)
制備方法

120484-50-6

93339-98-1
以2-氟-6-甲氧基苯乙酮為原料合成2-氟-6-羥基苯乙酮的一般步驟:向中間體3(9.0 g,53.5 mmol)在二氯甲烷(70 mL)中的冰冷溶液中加入氯化鋁(14.3 g,0.107 mol),隨后將反應混合物緩慢升溫至室溫。反應進行12小時后,用2N鹽酸水溶液淬滅反應,并用乙酸乙酯萃取。有機層依次用水洗滌,無水硫酸鈉干燥,減壓濃縮,得到2-氟-6-羥基苯乙酮,為棕色液體(5.48 g,收率66%)。產(chǎn)物經(jīng)核磁共振氫譜(1H NMR,CDCl3,400 MHz)確認:δ 12.72(s,1H,OH),7.40(m,1H,Ar-H),6.78(d,J = 8.5 Hz,1H,Ar-H),6.62(dd,J = 11.3,8.3 Hz,1H,Ar-H),2.69(d,J = 7.2 Hz,3H,CH3)。
參考文獻:
[1] Patent: WO2012/151525, 2012, A1. Location in patent: Page/Page column 101
[2] Patent: US2012/289496, 2012, A1. Location in patent: Page/Page column 100
[3] Patent: US5399584, 1995, A
[4] Patent: US2007/14733, 2007, A1. Location in patent: Sheet 14
[5] Bioorganic and Medicinal Chemistry Letters, 2012, vol. 22, # 1, p. 619 - 622