103068-40-2
103068-40-2 結(jié)構(gòu)式
基本信息
2-Fluoro-1,3-benzenediol
1,3-Benzenediol, 2-fluoro-
2-fluoro-1,3-dihydroxybenzene
物理化學(xué)性質(zhì)
制備方法
447462-87-5
103068-40-2
BBr3去甲基化的一般步驟:在氮?dú)獗Wo(hù)下,將2-氟-3-甲氧基苯酚(8.7毫摩爾)溶于干燥的二氯甲烷(40毫升)中,冷卻至-78℃。緩慢滴加BBr3(在二氯甲烷中1M溶液,每個(gè)甲氧基4當(dāng)量)。反應(yīng)混合物在-78℃下攪拌過(guò)夜,期間允許冷卻浴自然升溫至室溫。反應(yīng)完成后,將混合物再次冷卻至-78℃,并小心滴加水淬滅反應(yīng)。用EtOAc萃取水層,合并有機(jī)層,用無(wú)水Na2SO4干燥。減壓蒸發(fā)溶劑,得到粗產(chǎn)物。粗產(chǎn)物用EtOAc研磨,得到2-氟-1,3-苯二酚,無(wú)需進(jìn)一步純化即可用于后續(xù)反應(yīng)。該方法產(chǎn)率為93%。質(zhì)譜(MS)數(shù)據(jù):m/z 129.1(MH+)。
參考文獻(xiàn):
[1] Patent: US2009/298820, 2009, A1. Location in patent: Page/Page column 34
[2] Patent: WO2010/30727, 2010, A1. Location in patent: Page/Page column 92-93
[3] Patent: EP3401309, 2018, A1. Location in patent: Paragraph 0505
[4] Patent: US2009/311217, 2009, A1. Location in patent: Page/Page column 51
[5] Patent: WO2006/57860, 2006, A1. Location in patent: Page/Page column 114-115
