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hedanfeng鐵桿木蟲 (正式寫手)
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[求助]
真心請大神幫翻譯，偶翻譯的怕不準(zhǔn)確——3段有機合成步驟
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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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2樓2013-01-06 13:44:29
hedanfeng
鐵桿木蟲 (正式寫手)
- 應(yīng)助: 13 (小學(xué)生)
- 金幣: 6702.7
- 散金: 1927
- 紅花: 2
- 帖子: 956
- 在線: 331.7小時
- 蟲號: 194672
- 注冊: 2006-02-23
- 專業(yè): 無機材料化學(xué)
3樓2013-01-06 15:38:34
hedanfeng
鐵桿木蟲 (正式寫手)
- 應(yīng)助: 13 (小學(xué)生)
- 金幣: 6702.7
- 散金: 1927
- 紅花: 2
- 帖子: 956
- 在線: 331.7小時
- 蟲號: 194672
- 注冊: 2006-02-23
- 專業(yè): 無機材料化學(xué)
4樓2013-01-07 11:12:40
【答案】應(yīng)助回帖
★ ★
phu_grassman: 金幣+2, thanks for your time. 2013-01-07 12:51:04
phu_grassman: 金幣+2, thanks for your time. 2013-01-07 12:51:04
| -60 ℃，氮氣保護下，向三聚茚1 (2.2 g, 6.5 mmol)的四氫呋喃(70 mL)懸濁液中加入滴加正丁基鋰(2.5 M solution in n-hexane, 10.0 mL, 25.0 mmol)，約20 min。滴加完畢，升至室溫，然后室溫攪拌半小時。降至-60 ℃，滴加碘甲烷 (1.6 mL, 25.0 mmol)，緩慢升至室溫，室溫攪拌4小時。降溫至-60 ℃， 滴加正丁基鋰(2.5 M solution in n-hexane, 10.0 mL, 25.0 mmol)，攪拌2小時，滴加溴乙烷(1.6 mL, 25.0 mmol)，室溫攪拌12小時。將反應(yīng)液倒入水中，用二氯甲烷萃取，除去溶劑，柱層析（洗脫劑：石油醚） 后得到黃色粉末化合物1(2.6 g, 88%) . |
5樓2013-01-07 12:01:19
6樓2013-01-07 12:01:38
hedanfeng
鐵桿木蟲 (正式寫手)
- 應(yīng)助: 13 (小學(xué)生)
- 金幣: 6702.7
- 散金: 1927
- 紅花: 2
- 帖子: 956
- 在線: 331.7小時
- 蟲號: 194672
- 注冊: 2006-02-23
- 專業(yè): 無機材料化學(xué)
7樓2013-01-07 13:21:28
 |
8樓2013-01-07 19:49:16
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