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hedanfeng铁杆木虫 (正式写手)
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[求助]
真心请大神帮翻译，偶翻译的怕不准确——3段有机合成步骤
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1)To a stirred suspension of truxene1 (2.2 g, 6.5 mmol) in dry THF (70 mL) under nitrogen, n-BuLi (2.5 Msolution in n-hexane, 10.0 mL, 25.0 mmol) was added over a 20 min period at –60 ºC. Then the solutionwas warmed to room temperature aturally and stirred an additional half an hour at room temperature.Subsequently, Iodomethane (1.6 mL, 25.0 mmol) was added at –60 ºC, and then allowed the reaction mixture to come to room temperature slowly. After stirring for 4 h at room temperature the reaction mixture was cooled again to –60 ºC and a second portion of n-BuLi (2.5 M solution in n-hexane, 10.0 mL, 25.0 mmol) was added and in 2 h the second portion of bromoethane (1.6 mL, 25.0 mmol) was added. After stirring for 12 h at room temperature, the mixture was poured into water and extracted with dichloromethane. Removing the solvent, the crude product was afforded, which was purified by column chromatography on silica gel, eluting with petroleum ether and yielding compound 1 (2.6 g, 88%) as a yellow powder. 2) To a stirred solution of 1 (2.6 g, 6.1 mmol) in dichloromethane (70 mL), bromine was added (1.2 mL) at 0 °C free from light and left stirring at room temperature for 12 h in dark. Then washed the reaction mixture with 5% sodium bicarbonate solution (3 times), followed by water (1 time) and drying over magnesium sulfate, after removing solvent afforded of crude product. After purified by repeated washing with methanol the light yellow product was dried under vacuum (3.8 g, 91%). 3) 2,7,12-Tribromo-5,5,10,10,15,15-hexaethyltruxene (2) (2.5 g, 3.8 mmol) was dissolved in dry THF (80 mL) and the solution was cooled to -60 ºC. n-Butyllithium solution in n-hexane (2.5 M solution, 6.0 mL, 15.0 mmol) was syringed in with stirring under argon atmosphere at the low temperature. The reaction was stirred with cooling for 5 h to obtain a white thick suspension. Pure and dry carbon dioxide gas was continuously bubbled through the stirred mixture for 1 h at low emperature and an additional 1 h with the cooling bath removed to yield white thick slurry. Water (100 cm3) was added and the solution was acidified (pH ca. 1) using conc. HCl. The mixture was partitioned and the aqueous phase was extracted once with diethyl ether (50 cm3). After removal of ether in vacuum the white solid residue was repeatedly washed with hexane-chloroform mixture (5:2), finally recrystallised from MeOH–H2O to afford compound 3 as white powder (1.44 g, 79%). |
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hedanfeng
铁杆木虫 (正式写手)
- 应助: 13 (小学生)
- 金币: 6702.7
- 散金: 1927
- 红花: 2
- 帖子: 956
- 在线: 331.7小时
- 虫号: 194672
- 注册: 2006-02-23
- 专业: 无机材料化学
7楼2013-01-07 13:21:28
【答案】应助回帖
★ ★
phu_grassman: 金币+2, thanks for your time. 2013-01-07 12:51:04
phu_grassman: 金币+2, thanks for your time. 2013-01-07 12:51:04
| -60 ℃，氮气保护下，向三聚茚1 (2.2 g, 6.5 mmol)的四氢呋喃(70 mL)悬浊液中加入滴加正丁基锂(2.5 M solution in n-hexane, 10.0 mL, 25.0 mmol)，约20 min。滴加完毕，升至室温，然后室温搅拌半小时。降至-60 ℃，滴加碘甲烷 (1.6 mL, 25.0 mmol)，缓慢升至室温，室温搅拌4小时。降温至-60 ℃， 滴加正丁基锂(2.5 M solution in n-hexane, 10.0 mL, 25.0 mmol)，搅拌2小时，滴加溴乙烷(1.6 mL, 25.0 mmol)，室温搅拌12小时。将反应液倒入水中，用二氯甲烷萃取，除去溶剂，柱层析（洗脱剂：石油醚） 后得到黄色粉末化合物1(2.6 g, 88%) . |
5楼2013-01-07 12:01:19
6楼2013-01-07 12:01:38