1197953-47-1
1197953-47-1 結(jié)構(gòu)式
基本信息
2-(二甲基氧磷基)苯胺
2-(二甲基氧膦基)苯胺
2-(二甲基氧化磷基)苯胺
2-(二甲基亞膦?;?苯胺
(2-氨基苯基)二甲基氧化膦
(2-氨基苯基)二甲基膦氧化
2-(二甲基氧磷基)苯胺鹽酸鹽
2-(Dimethylphosphinyl)aniline
2-(diMethylphosphoryl)aniline
2-(diMethylphosphoryl)benzenaMine
2-(Dimethylphosphinyl)benzenamine
2-(diMethylphosphoryl)aniline HCl
2-(Dimethylphosphinyl)benzeneamine
Benzenamine, 2-(dimethylphosphinyl)-
(2-AMinophenyl)diMethylphosphine oxide
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法
615-43-0
7211-39-4
1197953-47-1
步驟1:化合物1的合成 在氮?dú)獗Wo(hù)下,向干燥的反應(yīng)瓶中加入2-碘苯胺(1.0當(dāng)量)、二甲基氧化膦(1.1當(dāng)量)和DMF作為溶劑。隨后加入磷酸鉀(1.1當(dāng)量)和乙酸鈀/Xantphos(催化量)。將反應(yīng)混合物在150℃下攪拌反應(yīng)3小時(shí),然后冷卻至室溫。減壓蒸餾除去DMF,殘余物用二氯甲烷和水進(jìn)行萃取分離。有機(jī)相經(jīng)無(wú)水硫酸鈉干燥后,濃縮得到粗產(chǎn)物。粗產(chǎn)物通過(guò)硅膠柱色譜法(洗脫劑:乙酸乙酯/甲醇=10:1)純化,得到化合物1,為棕色固體,收率80%。
參考文獻(xiàn):
[1] Patent: WO2012/151561, 2012, A1. Location in patent: Page/Page column 37
[2] Patent: WO2013/169401, 2013, A1. Location in patent: Page/Page column 41-42
[3] Patent: US2015/225436, 2015, A1. Location in patent: Paragraph 0791-0792
[4] Patent: CN106928275, 2017, A. Location in patent: Paragraph 0097-0099
[5] Journal of Medicinal Chemistry, 2016, vol. 59, # 10, p. 4948 - 4964
