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團(tuán)子小姐新蟲(chóng) (初入文壇)
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[求助]
論文翻譯,英語(yǔ)論文翻譯
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Diphenylamine (3.4 g, 20 mmol) potassium tert-butoxide(0.43 g, 4.5 mmol), Pd(dppf)Cl2 (0.15 mmol), dppf (1 mmol)and dried toluene (60 mL) were mixed in a three-necked flask.The mixture was heated at 70 Cfor10minwiththeaddition of 4-bromobenzophenone (5.2 g, 20 mmol). The resulting mixture was vigorously stirred for 24 h at 120 ??C. After the reaction finished, a certain amount of hydrochloric acid was slowly added. Subsequently, the residue was extracted with dichloromethane. The extraction solution was washed with brine, and then the organic layer was dried over MgSO4 and filtered. The crude product was purified by column chromatography using a dichloromethane?Chexane (1/50) mixture as eluent to obtain the desired compound in 44.2% yield (3.1 g);1HNMR(500MHz,CDCl3) d 7.79 (d, J = 7.0 Hz, 2H), 7.72 (dd,J =7.0 Hz, J = 1.5 Hz, 2H), 7.56 (t, J = 7.5 Hz, 1H), 7.48 (t, J =7.5 Hz, 2H), 7.35 (t, J = 9.0 Hz, 4H), 7.20 (d, J =7.5 Hz, 4H), 7.16 (t, J = 7.5 Hz, 2H), 7.03 (dd, J = 7.0 Hz, J = 2.0 Hz, 2H).13CNMR (500 MHz, CDCl3); d 195.2, 151.9, 146.5, 138.5, 131.9, 131.7, 129.6, 128.1, 126.0, 124.6, 119.6; crystallographic data for TPA-CO:C25H19NO, M = 349.41, orthorhombic, a =16.740(5) ˚ A, b = 12.432(5) ˚ A, c = 9.236(3) ˚ A; V = 1922.2(11) ˚ A3,T = 296(2) K, space group Pca2(1), DC = 1.207 g cmˆ??3, Z = 4,10 430 reflections collected, 3385 unique reflection (Rint =0.0308), the final R indices were R1=0.0384, wR2 = 0.0799 [I >2??(I)], CCDC=872836. |
至尊木蟲(chóng) (著名寫(xiě)手)
| 在三頸燒瓶中,加入二苯胺(3.4克,20 mmol)、叔丁醇鉀(0.43克,4.5 mmol)、Pd(dppf)Cl2(0.15 mmol)、dppf(1 mmol)和干燥的甲苯(60 ml)。加入4-溴苯二酮(5.2克,20 mmol),在70℃加熱混合液10分鐘。在120℃用力攪拌得到的混合液24小時(shí)。反應(yīng)結(jié)束后,緩慢加入一定量的鹽酸。然后用二氯甲烷萃取殘留物。用鹽水沖洗萃取液,然后用硫酸鎂干燥有機(jī)層,并過(guò)濾。使用二氯甲烷-己烷(1/50)作為洗脫劑通過(guò)柱色譜法純化粗品得到目標(biāo)化合物,收率為44.2%(3.1克);后面的是核磁數(shù)據(jù)和晶體數(shù)據(jù)了~~~就不一一譯了~~~ |

鐵桿木蟲(chóng) (文壇精英)

至尊木蟲(chóng) (著名寫(xiě)手)

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