|
|
【答案】应助回帖
★ ★ ★ ★ ★ ★ 真强必胜: 金币+1, ? 2014-09-22 18:26:27 zhangwei章薇: 金币+5, 翻译EPI+1, 一些化学专用单词都没有翻译出来,不过还是谢谢帮助我的人 2014-09-23 13:27:51
合成 2,6-bis(diethylphosphorylmethyl)-9,10-distyrylanthracene
高压反应管内加入苯乙烯 (1.11 g, 10.1 mmol), 2,6-bis(diethylphosphorylmethyl)-9,10-dibromoanthracene (1.35g, 2.13 mmol), Pd(OAc)2 (52 mg, 0.21 mmol), tri(o-tolyl) phosphine (0.38 g, 1.21 mmol), N(C2H5)3 (7 mL) and THF (7mL) ,氮气保护下。螺旋特氟龙盖密封。80度回流24小时,冷却,溶剂蒸发,残留物硅胶柱层析分离提纯, 洗脱液乙酸乙酯-正己烷(3:1)收率: 1.16 g (80.6%). 核磁数据: 1H NMR (500 MHz, CDCl3, δ): 8.35 (d, J ¼ 9 Hz, 2H), 8.21 (s, 2H), 7.89 (d, J ¼ 11.5 Hz, 2H), 7.69 (d, J ¼ 7.5 Hz, 4H), 7.48 (m, 6H), 7.39 (m, 2H), 6.92 (d, J ¼17 Hz, 2H), 4.03 (m, 8H), 3.33 (d, 4H), 1.23 (m, 12H). 元素分析Anal. calcd for C40H44O6P2: C, 70.37; H, 6.50; O, 14.06; P, 9.07. Found: C, 70.46; H, 6.44 |
|