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清風拂夢新蟲 (小有名氣)
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[求助]
求翻譯以下一段話！謝謝！材料化學類的
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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】應助回帖
★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★
真強必勝: 金幣+1, 謝謝 2014-11-11 19:02:59
清風拂夢: 金幣+10, ★★★很有幫助 2014-11-18 00:04:53
真強必勝: 金幣+1, 謝謝 2014-11-11 19:02:59
清風拂夢: 金幣+10, ★★★很有幫助 2014-11-18 00:04:53
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化合物2（6.0克，9.010 3 摩爾）溶于無水四氫呋喃（100毫升）中，冷卻至-78攝氏度，然后正丁基鋰（2.2 M的正丁烷溶液, 6 毫升, 0.0132 摩爾）在氬氣保護下在-78攝氏度下滴入上述溶液中。然后攪拌5小時，硼酸三甲酯（2.2毫升）在-78度下快速加入，反應混合物慢慢升至室溫，攪拌過夜。然后混合物用2M的鹽酸酸化2小時。然后反應混合物用二氯甲烷攝取三次（每次用50毫升），有機相用無水硫酸鈉干燥。有機溶劑減壓蒸餾除掉，粗品用硅膠柱純化（流動相：丙酮：二氯甲烷=1：20 體積比）得到3（2.1克，收率：55%），氫譜（300兆，氘化二甲亞砜作溶劑）：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)；質(zhì)譜：m/ z: 586 ([M-(B(OH)2)] + , 計算值C44H29, 585); 元素分析：計算值C44H31BN2O2: C 83.81, H 4.96, N 4.44; 測得值: C 83.64, H 4.89, N 4.48. |
2樓2014-11-11 09:23:47
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