103291-07-2

基本信息
5-溴-2-氟甲氧基苯
4-氟-3-甲氧基溴苯
2-氟-5-溴苯甲醚 100G
2-fluoro-5-bromoanisole
2-FLUORO-5-BROMO ANISOLE,=98%
4-Bromo-1-fluoro-2-methoxybenzene
Benzene,4-broMo-1-fluoro-2-Methoxy
4-Bromo-1-fluoro-2-methoxybenzene, 5-Bromo-2-fluorophenyl methyl ether
物理化学性质
制备方法

112204-58-7

74-88-4

103291-07-2
以5-溴-2-氟苯酚(13.0g,68.1mmol)和碘甲烷(19.3g,136mmol)为原料,在DMF(120mL)中溶解后,加入碳酸钾(18.8g,136mmol)。反应混合物在室温下搅拌65小时。反应完成后,向反应液中加入水(150mL),用乙酸乙酯(100mL×1,50mL×2)进行萃取。合并有机层,用无水硫酸镁干燥,减压浓缩,得到淡黄色油状粗产物(29.0g)。粗产物通过硅胶柱色谱法(洗脱剂:己烷/乙酸乙酯=10:1)纯化,得到无色油状的5-溴-2-氟苯甲醚(14.2g,收率:定量)。产物结构经1H-NMR(400MHz,CDCl3)和19F-NMR(376MHz,CDCl3)确认:1H-NMR δ 3.88(s,3H),6.95(dd,J = 8.6和10.8Hz,1H),7.02(ddd,J = 2.2,4.2和8.6Hz,1H),7.08(dd,J = 2.2和7.6Hz,1H);19F-NMR δ -137(s,1F)。
参考文献:
[1] Patent: US2016/24110, 2016, A1. Location in patent: Paragraph 0452; 0453
[2] Patent: WO2006/76246, 2006, A2. Location in patent: Page/Page column 87
[3] Patent: US2010/227894, 2010, A1. Location in patent: Page/Page column 28
[4] Patent: US2007/3539, 2007, A1. Location in patent: Page/Page column 71