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[求助]
求翻译以下一段话！谢谢！材料化学类的
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Compound2(6.0 g, 9.010 3 mol) was dissolved in anhydrous THF (100 mL) andn-butyllithium (2.2 M/hexane, 6 mL, 0.0132 mol) was added, dropwise, under an argon atomosphere at 78 C. After stirring for 5 h, B(OCH3)3 (2.2 mL) was added quickly at78 C and the mixture was stirred overnight allowing the temperature to rise gradually to room temperature. Then, the reaction mixture was acidified with hydrochloric acid (2 M) for 2 h. The mixture was extracted with dichloromethane (3 50 mL) and the organic layer was dried with anhydrous sodium sulfate. After removing the solvent under reduced pressure, the crude product was purified by silica gel column chromatography using acetone/CH2Cl2 (1 : 20, v) as eluent to yield 3(2.1 g, yield 55%). 1 H-NMR (300 MHz, DMSO-d6) d: 7.137 (s, 1H, >C]CH–), 7.25–7.58 (m, 16 H), 7.62–7.78 (m, 8 H), 7.976 (s, 2 H, –B(OH)2), 8.20–8.30 (m, 4 H, carbazole–H); MS (EI),m/ z: 586 ([M-(B(OH)2)] + , calcd for C44H29, 585); anal. calc. For C44H31BN2O2: C 83.81, H 4.96, N 4.44; found: C 83.64, H 4.89, N 4.48. |
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【答案】应助回帖
★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★
真强必胜: 金币+1, 谢谢 2014-11-11 19:02:59
清风拂梦: 金币+10, ★★★很有帮助 2014-11-18 00:04:53
真强必胜: 金币+1, 谢谢 2014-11-11 19:02:59
清风拂梦: 金币+10, ★★★很有帮助 2014-11-18 00:04:53
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化合物2（6.0克，9.010 3 摩尔）溶于无水四氢呋喃（100毫升）中，冷却至-78摄氏度，然后正丁基锂（2.2 M的正丁烷溶液, 6 毫升, 0.0132 摩尔）在氩气保护下在-78摄氏度下滴入上述溶液中。然后搅拌5小时，硼酸三甲酯（2.2毫升）在-78度下快速加入，反应混合物慢慢升至室温，搅拌过夜。然后混合物用2M的盐酸酸化2小时。然后反应混合物用二氯甲烷摄取三次（每次用50毫升），有机相用无水硫酸钠干燥。有机溶剂减压蒸馏除掉，粗品用硅胶柱纯化（流动相：丙酮：二氯甲烷=1：20 体积比）得到3（2.1克，收率：55%），氢谱（300兆，氘化二甲亚砜作溶剂）：d: 7.137 (s, 1H, >C]CH–), 7.25–7.58 (m, 16 H), 7.62–7.78 (m, 8 H), 7.976 (s, 2 H, –B(OH)2), 8.20–8.30 (m, 4 H, carbazole–H)；质谱：m/ z: 586 ([M-(B(OH)2)] + , 计算值C44H29, 585); 元素分析：计算值C44H31BN2O2: C 83.81, H 4.96, N 4.44; 测得值: C 83.64, H 4.89, N 4.48. |
2楼2014-11-11 09:23:47
