627899-90-5
627899-90-5 结构式
基本信息
4-[3-(二甲胺基)丙氧基]苯硼酸频哪醇酯
4-[3-(二甲基氨基)丙氧基]苯基硼酸频哪醇酯
2-(4-[3-(二甲基氨基)丙氧基]苯基)-4,4,5,5-四甲基-1,3,2-二氧杂硼烷
N,N-二甲基-3-(4-(4,4,5,5-四甲基-1,3,2-二氧硼杂环戊烷-2-基)苯氧基)丙-1-胺
4-[3-(Dimethylamino)propoxy]benzene boronic acid, pinacol ester
2-{4-[3-(dimethylamino)propoxy]phenyl}-4,4,5,5-tetramethyl-1,3,2-dioxaborolane
N,N-dimethyl-3-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenoxy]1-Propanamine
N,N-Dimethyl-3-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenoxy]propan-1-amine
1-Propanamine, N,N-dimethyl-3-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenoxy]-
制备方法
76579-64-1
61676-62-8
627899-90-5
一般步骤:向100 mL经火焰干燥的两颈烧瓶中加入3-(4-溴苯氧基)-N,N-二甲基-1-丙胺(3.0 g,11.6 mmol)和新蒸馏的四氢呋喃(80 mL)。将所得溶液冷却至-78℃,在氮气保护下,于10分钟内滴加正丁基锂(8.7 mL,13.9 mmol,1.6 M己烷溶液)。将反应混合物在-78℃下搅拌1小时。随后,迅速加入异丙醇频哪醇硼酸酯(2.6 g,13.9 mmol),并将所得混合物缓慢升温至室温,持续反应24小时。反应完成后,将混合物倒入50 mL水中,用氯仿(300 mL)萃取。合并有机层,用饱和食盐水洗涤,无水硫酸镁干燥。通过旋转蒸发去除溶剂,残余物经硅胶柱色谱纯化(洗脱剂:乙酸乙酯/二氯甲烷),得到目标产物为浅黄色油状物(1.6 g,收率:45.0%)。产物表征数据如下:1H NMR (400 MHz, CDCl3, Me4Si): δ = 7.77 (d, 2H, J = 8.8 Hz), 6.90 (d, 2H, J = 8.8 Hz), 3.94 (t, 2H, J = 6.4 Hz), 2.46 (t, 2H, J = 6.8 Hz), 2.26 (s, 6H), 1.88 (m, 2H, J = 6.8 Hz), 1.25 (s, 12H)。13C NMR (100 MHz, CDCl3, Me4Si): 161.57, 136.73, 113.41, 83.13, 74.40, 66.02, 54.09, 45.42, 27.43, 25.00。元素分析计算值(C17H28BNO3):C, 66.90; H, 9.25; N, 4.59。实测值:C, 66.73; H, 9.23; N, 4.63。IR (KBr, cm-1): 2981, 2936, 2816, 2716, 1566, 1463, 1281, 1245。
参考文献:
[1] Dyes and Pigments, 2015, vol. 113, p. 210 - 218
[2] Patent: KR2015/122308, 2015, A. Location in patent: Paragraph 0094; 0095; 0098; 0099

