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英语翻译1,3,5-Tris((3-(5¢-n-hexyl-2,2¢-bipyridin-5-yl)

来源:学生作业帮 编辑:作业帮 分类:化学作业 时间:2024/10/01 22:04:14
英语翻译
1,3,5-Tris((3-(5¢-n-hexyl-2,2¢-bipyridin-5-yl)ethynyl)-
bicyclo[1.1.1]pent-1-ylethynyl)benzene (4).In a two-neck
flask,22 (124 mg,0.350 mmol) and 1,3,5-triiodobenzene (54
mg,0.119 mmol) were combined,evacuated,and put under
argon.Freshly distilled dry piperidine (20 mL) was added from
a syringe,and the mixture was stirred at room temperature
until the solid was dissolved.Then,the solution was degassed
by three freeze-pump-thaw cycles.After warming to room
temperature,Pd(PPh3)4 (10 mg,2.5 mol %) was added from a
tip tube,and the reaction mixture was stirred at 55 °C for 24
h.Aqueous NaOH (4 M,2.5 mL) was added,and the solution
was stirred for 15 min before the solvents were evaporated
under reduced pressure.The crude solid was dissolved in
chloroform and washed with aqueous EDTA solution (1 M,3
\2 5 mL).After drying over Na2SO4,the organic solvent was
evaporated under reduced pressure,and the crude product was
purified by PTLC (alumina,hexane/ethyl acetate,5:1) to yield
4 as a white solid:95 mg (71%); mp 169 °C (dec); 1H NMR
(CDCl3,500 MHz) ä 0.86 (t,J ) 7.3 Hz,9 H),1.31 (m,18 H),
1.60 (m,6 H),2.46 (s,18 H),2.63 (t,J ) 7.7 Hz,6 H),7.36 (s,
3 H),7.59 (dd,J ) 8.1 Hz,J ) 1.8 Hz,3 H),7.77 (dd,J ) 8.3
Hz,J ) 2.0 Hz,3 H),8.27 (d,J ) 8.4 Hz,3 H),8.29 (d,J ) 8.4
Hz,3 H),8.47 (d,J ) 1.6 Hz,3 H),8.66 (d,J ) 1.6 Hz,3 H);
13C {1H} NMR (CDCl3,124 MHz) ä 14.05,22.55,28.77,30.79,
31.01,31.59,32.86,58.96,77.43,78.70,89.15,92.13,119.51,
119.94,120.94,123.41,134.36,136.77,138.59,139.55,149.41,
151.75,153.10,154.94; IR (KBr) 652,682,742,835,878,1024,
1053,1208,1283,1384,1417,1464,1538,1585,2854,2924,
2955 cm-1; MS (ESI+) m/z (rel int) 1158 ([M + Na]+,5),1136
([M + H]+,100),568 ([M + 2H]2+,50).Anal.Calcd.for
C81H78N6:C,85.68; H,6.93; N,7.40.Found:C,85.57; H,7.18;
N,7.27.
1,3,5三( ( 3 - ( 5 ¢ - N -已基- 2 ,2 ¢ - bipyridin - 5 -基)乙炔) -
双环[ 1.1.1 ]压抑- 1 - ylethynyl )苯( 4 ) .在两颈部
瓶,22 ( 124毫克,0.350浓度)和1,3,5 triiodobenzene ( 54
毫克,0.119浓度)相结合,疏散,并根据
氩气.新鲜蒸馏干哌啶( 20毫升)加入从
注射器和混合物是在室温下搅拌
直到固体被解散.然后,该解决方案是脱气
由三个冷冻泵冻融周期.在气候变暖室
温度,钯(三苯基膦) 4 ( 10毫克,2.5摩尔% )增加了
尖管,反应混合物被搅动在55 ℃时为24
阁下氢氧化钠水溶液( 4男,2.5毫升)加入,并解决
被激起的15分钟之前,溶剂蒸发
根据减少的压力.原油固体被解散
氯仿和冲洗水EDTA溶液( 1男,3
5毫升) .干燥后的硫酸钠,有机溶剂
蒸发减少压力下,以及原油产品
纯化PTLC (氧化铝,正己烷/乙酸乙酯,5时01分) ,收益率
4作为一种白色固体:95毫克( 71 % ) ;熔点169 ℃ ( 12月) ;的1H NMR
( CDCl3 ,500兆赫)在0.86的( t ,J )条7.3赫兹,9 h )下,1月31日(男,18 h )下,
1.60 (男,6小时) ,2.46 (秒,18个高) ,2.63 (吨,强) 7.7赫兹,6小时) ,7.36 (秒,
3小时) ,7.59 (日,强) 8.1赫兹,强) 1.8赫兹,3小时) ,7.77 (日,强) 8.3
赫兹,强) 2.0赫兹,3小时) ,8月27日(四,强) 8.4赫兹,3小时) ,8月29日(四,强) 8.4
赫兹,3小时) ,8.47 (四,强) 1.6赫兹,3小时) ,8.66 (四,强) 1.6赫兹,3小时) ;
( )的13C核磁共振氢( CDCl3 ,124兆赫)在5月14日,22.55 ,28.77 ,30.79 ,
31.01 ,31.59 ,32.86 ,58.96 ,77.43 ,78.70 ,89.15 ,92.13 ,119.51 ,
119.94 ,120.94 ,123.41 ,134.36 ,136.77 ,138.59 ,139.55 ,149.41 ,
151.75 ,153.10 ,154.94 ;红外(溴化钾) 652 ,682 ,742 ,835 ,878 ,1024 ,
1053年,1208年,1283年,1384年,1417年,1464年,1538年,1585年,2854年,2924年,
二九五五厘米- 1 ;毫秒(喷雾+ )米/环Z (相对国际) 1158 ( [的M +钠] + ,5 ) ,1136
( [的M + H ]条+ ,100 ) ,568 ( [的M +下半年] 2 + ,50 ) .肛门.Calcd .为了
C81H78N6 :ć ,85.68 ;小时,6.93 ;氮,7.40 .发现:ć ,85.57 ;小时,7月18日;
氮,7月27日.