英语翻译1,2,4,5-Tetra((3-(2,2¢-bipyridin-5-yl)ethynyl)bicyclo-[1.1.1]pent-1-ylethynyl)benzene (7).A 25 mL two-neckflask was charged with 20 (309 mg,1.14 mmol) and 1,2,4,5-tetraiodobenzene (158 mg,0.272 mmol),evacuated,and filledwith argon.Dr
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英语翻译1,2,4,5-Tetra((3-(2,2¢-bipyridin-5-yl)ethynyl)bicyclo-[1.1.1]pent-1-ylethynyl)benzene (7).A 25 mL two-neckflask was charged with 20 (309 mg,1.14 mmol) and 1,2,4,5-tetraiodobenzene (158 mg,0.272 mmol),evacuated,and filledwith argon.Dr
英语翻译
1,2,4,5-Tetra((3-(2,2¢-bipyridin-5-yl)ethynyl)bicyclo-
[1.1.1]pent-1-ylethynyl)benzene (7).A 25 mL two-neck
flask was charged with 20 (309 mg,1.14 mmol) and 1,2,4,5-
tetraiodobenzene (158 mg,0.272 mmol),evacuated,and filled
with argon.Dry piperidine (10 mL) was added from a syringe,
and the solution was degassed by three freeze-pump-thaw
cycles.Then,Pd(PPh3)4 (33 mg,2.5 mol %) was added from a
tip tube,and the reaction mixture was stirred for 6 days at 50
°C.Additional Pd(PPh3)4 (18 mg,1.25 mol %) was added from
a tip tube,and the reaction was continued for 5 more days.
Then,NaOH (4 M in water,5 mL) was added,and the mixture
was stirred for 10 min.The solvents were removed under
reduced pressure,and chloroform was added.The organic layer
was washed with EDTA (1 M,3 \2 10 mL),dried over Na2SO4,
and evaporated under reduced pressure.The crude product
mixture was separated by HPLC (C18,acetonitrile/chloroform-
2.5% Et3N),and 7 was obtained as an off-white solid:174 mg
(56%); mp 212 °C (dec); 1H NMR (CDCl3,500 MHz) ä 2.51 (s,
12 H),7.29 (dd,J ) 6.8 Hz,J ) 4.9 Hz,2 H),7.41 (s,1 H),
7.78 (td,J ) 8.1 Hz,J ) 1.8 Hz,2 H),7.79 (dd,J ) 8.4 Hz,J
) 1.8 Hz,2 H),8.32 (d,J ) 8.4 Hz,2 H),8.32 (d,J ) 8.1 Hz,
2 H),8.64 (d,J ) 3.2 Hz,2 H),8.66 (s,2 H); 13C {1H} NMR
(CDCl3,124 MHz) ä 31.20,31.32,59.38,77.78,78.23,92.49,
94.19,120.13,120.54,121.61,124.19,125.41,135.11,137.22,
139.89,149.52,152.08,155.05,155.70; IR (KBr) 534,614,652,
694,731,747,796,856,899,992,1021,1038,1091,1120,1225,
1241,1260,1288,1369,1384,1433,1457,1486,1543,1571,
1586,2225,2876,2913,2987,3048 cm-1; MS (FAB+/3-NOBA)
m/z 1151 ([M + H]+); MS (ESI -) m/z 1151 ([M + H]+).Anal.
Calcd for C82H54N8:C,85.54; H,4.73.Found:C,85.88; H,
4.92.
英语翻译1,2,4,5-Tetra((3-(2,2¢-bipyridin-5-yl)ethynyl)bicyclo-[1.1.1]pent-1-ylethynyl)benzene (7).A 25 mL two-neckflask was charged with 20 (309 mg,1.14 mmol) and 1,2,4,5-tetraiodobenzene (158 mg,0.272 mmol),evacuated,and filledwith argon.Dr
1,2,4,5 -四( ( 3 - ( 2,2 ¢ - bipyridin - 5 -基)乙炔)双环-
[ 1.1.1 ]压抑- 1 - ylethynyl )苯( 7 ) .25毫升两个瓶颈
瓶被指控犯有20个( 309毫克,1月14日浓度)和1,2,4,5 -
tetraiodobenzene ( 158毫克,0.272浓度) ,疏散,并填补
氩.干哌啶( 10毫升)加入从注射器,
和脱气的解决办法是由三个冷冻泵解冻
周期.然后,钯(三苯基膦) 4 ( 33毫克,2.5摩尔% )增加了
尖管,反应混合物被搅动的6天,在50
° C的附加钯(三苯基膦) 4 ( 18毫克,1月25日摩尔% )增加了从
小费管,反应是持续了5天.
然后,氢氧化钠( 4米的水,5毫升)加入,并混合物
是搅拌10分钟.溶剂下被拆除
减少压力,增加了氯仿.有机层
洗涤用EDTA ( 1男,3月10日毫升) ,干多硫酸钠,
和蒸发压力下减少.原油产品
分离混合物的高效液相色谱( C18柱,acetonitrile/chloroform-
2.5 % Et3N ) ,7 ,获得一个类白色固体:174毫克
( 56 % ) ;熔点212 ℃ ( 12月) ;的1H NMR ( CDCl3 ,500兆赫)在2.51 (秒,
12小时) ,7月29日(日,强) 6.8赫兹,强) 4.9赫兹,2小时) ,7.41 (秒,1 h )下,
7.78 (运输署,强) 8.1赫兹,强) 1.8赫兹,2小时) ,7.79 (日,强) 8.4赫兹,强
) 1.8赫兹,2小时) ,8.32 (四,强) 8.4赫兹,2小时) ,8.32 (四,强) 8.1赫兹,
2小时) ,8.64 (四,强) 3.2赫兹,2小时) ,8.66 (秒,2小时) ;的13C ) (质子核磁共振
( CDCl3 ,124兆赫)在31.20 ,31.32 ,59.38 ,77.78 ,78.23 ,92.49 ,
94.19 ,120.13 ,120.54 ,121.61 ,124.19 ,125.41 ,135.11 ,137.22 ,
139.89 ,149.52 ,152.08 ,155.05 ,155.70 ;红外(溴化钾) 534 ,614 ,652 ,
694 ,731 ,747 ,796 ,856 ,899 ,992 ,1021年,1038年,1091年,1120年,1225年,
1241年,1260年,1288年,1369年,1384年,1433年,1457年,1486年,1543年,1571年,
1586年,2225年,2876年,2913年,2987年,三零四八厘米- 1 ;毫秒(轰击+ / 3 ,野场)
米/ Z用1151 ( [的M + H ]条+ ) ;毫秒(喷雾- )米/ ž 1151 ( [的M + H ]条+ ) .肛门.
Calcd为C82H54N8 :ć ,85.54 ;小时,4.73 .发现:ć ,85.88 ;小时,
4.92 .