62257-16-3

物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

84478-75-1

62257-16-3
以2-氯-4-氟-5-硝基苯酚為原料合成3-氨基-4-氟苯酚的一般步驟如下:將2-氯-4-氟-5-硝基苯酚(85g,0.45mol)與10%Pd/C催化劑(25g,0.023mol)在乙醇中混合,于50psi氫氣壓力下進(jìn)行氫化反應(yīng)12小時(shí)。反應(yīng)完成后,過(guò)濾去除催化劑,濾液經(jīng)減壓濃縮除去溶劑,所得粗產(chǎn)物通過(guò)硅膠柱色譜法純化,得到3-氨基-4-氟苯酚(40g,收率70%)。產(chǎn)物結(jié)構(gòu)經(jīng)1H NMR(400MHz,DMSO-d6)和質(zhì)譜(ESI)確認(rèn):1H NMR δ8.87(s,1H),6.70(dd,J = 11.2,8.8Hz,1H),6.14(dd,J = 7.8,2.4Hz,1H),5.84(m,1H),4.92(s,2H);MS(ESI)m/z:128.2(M + H+)。
參考文獻(xiàn):
[1] Organic Process Research and Development, 2014, vol. 18, # 1, p. 122 - 134
[2] Patent: US2008/90856, 2008, A1. Location in patent: Page/Page column 38
[3] Patent: WO2010/51373, 2010, A1. Location in patent: Page/Page column 75-76
[4] Patent: WO2013/36232, 2013, A2. Location in patent: Paragraph 00253
[5] Patent: US2009/137595, 2009, A1