74587-12-5

物理化學(xué)性質(zhì)
制備方法

5399-03-1

74587-12-5
以2-碘-4-硝基苯甲醚為原料合成3-碘-4-甲氧基苯胺的一般步驟:向250 mL圓底燒瓶中加入2-碘-1-甲氧基-4-硝基苯(6 g,21.50 mmol,1.00當(dāng)量)、鐵粉(3.61 g,64.50 mmol,3.00當(dāng)量)、氯化銨(3.42 g,63.94 mmol,3.00當(dāng)量)、乙醇(50 mL)和水(10 mL)。將反應(yīng)混合物在85℃下攪拌1小時。反應(yīng)完成后,過濾除去固體不溶物,并將濾液在減壓下濃縮。得到棕色固體產(chǎn)物3-碘-4-甲氧基苯胺(5.35 g,收率100%)。通過液相色譜-質(zhì)譜聯(lián)用(LC-MS)分析產(chǎn)物:(電噴霧離子化,m/z)保留時間(RT)= 0.847分鐘,LCMS 53:m/z = 250 [M + 1]。
參考文獻:
[1] Patent: WO2018/118842, 2018, A1. Location in patent: Paragraph 0421-0424
[2] Patent: WO2016/199943, 2016, A1. Location in patent: Paragraph 0303
[3] Patent: WO2013/14039, 2013, A1. Location in patent: Page/Page column 45-46
[4] Patent: WO2014/152029, 2014, A2. Location in patent: Paragraph 00230
[5] Journal of the American Chemical Society, 1941, vol. 63, p. 2482,2484