348-28-7

基本信息
4-氟水楊醛
4-FLUORO-2-HYDROXYBENZALDEHYDE
4-FLUOROSALICYLALDEHYDE
2-Hydroxy-4-Fluorobenzaldehyde 4-Fluoro Salicylaldehyde
4-FLUOROSALICYLALDEHYDE (4-FLUORO-2-HYDROXYBENZALDEHYDE)
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

50-00-0

372-20-3

348-28-7
以甲醛和3-氟苯酚為原料合成4-氟-2-羥基苯甲醛的一般步驟如下:向含有3-氟苯酚(5 mL,55.3 mmol)和無水乙腈(250 mL)的混合物中加入MgCl2(14.2 g,149 mmol)、無水三甲胺(27 mL)和多聚甲醛(11 g)。將反應(yīng)混合物在回流條件下攪拌5小時,隨后冷卻至室溫。反應(yīng)通過加入5%鹽酸(250 mL)淬滅,并用乙酸乙酯(100 mL × 3)進(jìn)行萃取。合并的有機(jī)層依次用5%鹽酸、水和鹽水洗滌,經(jīng)無水硫酸鈉干燥后,減壓濃縮。粗產(chǎn)物通過硅膠柱色譜純化(洗脫劑:石油醚/乙酸乙酯=50:1至20:1),得到4-氟-2-羥基苯甲醛(5 g,產(chǎn)率65%),為淺黃色固體。1H NMR(400 MHz,CDCl3)數(shù)據(jù)如下:δ 11.37(d,J = 1.6 Hz,1H),9.83(s,1H),7.55-7.59(m,1H),6.65-6.75(m,2H)。
參考文獻(xiàn):
[1] Patent: WO2004/87686, 2004, A2. Location in patent: Page 504
[2] Patent: WO2004/87687, 2004, A1. Location in patent: Page 504
[3] Patent: WO2017/55860, 2017, A1. Location in patent: Page/Page column 138-139
[4] Patent: US2017/37038, 2017, A1. Location in patent: Paragraph 0375; 0376; 0377
[5] Patent: KR101679262, 2016, B1. Location in patent: Paragraph 0156-0158