120100-15-4

基本信息
Benzoic acid, 3-amino-2-chloro-, methyl ester
物理化學(xué)性質(zhì)
制備方法

53553-14-3

120100-15-4
步驟B:3-氨基-2-氯苯甲酸甲酯的合成; 在2-氯-3-硝基苯甲酸甲酯(25g,116mmol)的甲醇(MeOH,150mL)溶液中加入Raney Ni催化劑(3g)。將反應(yīng)混合物置于氫氣氣氛(50psi,25℃)下攪拌反應(yīng)3.5小時(shí)。反應(yīng)完成后,過(guò)濾除去催化劑,濾液在減壓下濃縮至干,得到粗產(chǎn)物。粗產(chǎn)物通過(guò)乙酸乙酯(EtOAc)重結(jié)晶進(jìn)行純化,得到標(biāo)題化合物3-氨基-2-氯苯甲酸甲酯(合并四批,總產(chǎn)量69g,收率83.5%)。產(chǎn)物結(jié)構(gòu)經(jīng)1H NMR(400MHz,CDCl3)確認(rèn):δ 6.7-7.5.25(m,3H,芳烴H),4.40-4.50(br,2H,NH2),3.87(s,3H,OCH3)。
參考文獻(xiàn):
[1] Patent: JP2015/528022, 2015, A. Location in patent: Paragraph 0659
[2] Patent: WO2018/134254, 2018, A1. Location in patent: Page/Page column 64; 65
[3] Patent: US2009/298815, 2009, A1. Location in patent: Page/Page column 63
[4] Patent: WO2011/59610, 2011, A1. Location in patent: Page/Page column 97
[5] Patent: US6177440, 2001, B1