1590-25-6

基本信息
2-乙?;?6-溴萘
(6-bromo-2-naphthalenyl)ethanone
1-(6-Bromonaphthalen-2-yl)ethanone
1-(6-bromonaphthalen-2-yl)ethan-1-one
Ethanone, 1-(6-bromo-2-naphthalenyl)-
物理化學(xué)性質(zhì)
制備方法

861880-64-0

75-16-1

1590-25-6
在氮?dú)獗Wo(hù)下,將6-溴-N-甲氧基-N-甲基-2-萘甲酰胺(82.9 g,282 mmol,1.0當(dāng)量)溶解于四氫呋喃(600 mL)中,置于四頸燒瓶?jī)?nèi)。將反應(yīng)混合物置于冰浴中冷卻,控制溫度在10-15℃范圍內(nèi),緩慢滴加甲基溴化鎂(3.2 M,在甲基四氫呋喃中,197 mL,2.2當(dāng)量),滴加過(guò)程持續(xù)1小時(shí)。滴加完畢后,繼續(xù)在冰浴中攪拌反應(yīng)混合物30分鐘。隨后,在冰浴冷卻下,小心滴加2M鹽酸水溶液(100 mL)以淬滅反應(yīng)。蒸發(fā)除去有機(jī)溶劑后,用二氯甲烷(500 mL)萃取沉淀的產(chǎn)物。合并有機(jī)相,用無(wú)水硫酸鈉干燥,過(guò)濾后濃縮。將所得固體殘余物在40℃下真空干燥,得到1-(6-溴萘-2-基)乙酮(70.6 g,收率99%)。
參考文獻(xiàn):
[1] Patent: WO2011/54834, 2011, A1. Location in patent: Page/Page column 39
[2] Patent: WO2011/91446, 2011, A1. Location in patent: Page/Page column 11
[3] Patent: US2017/253614, 2017, A1. Location in patent: Paragraph 0574; 0575
[4] Patent: US2011/64695, 2011, A1. Location in patent: Page/Page column 94
[5] Patent: US2011/64697, 2011, A1. Location in patent: Page/Page column 85