英语翻译1,2,4,5-Tetra((3-(4-pyridyl)ethynyl)bicyclo[1.1.1]pent-1-ylethynyl)benzene (6).A 25 mL two-neck flask wascharged with 23 (113 mg,0.585 mmol) and 1,2,4,5-tetraiodobenzene(81 mg,0.139 mmol),evacuated,and filled with argon.Dry piperidine (15
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英语翻译1,2,4,5-Tetra((3-(4-pyridyl)ethynyl)bicyclo[1.1.1]pent-1-ylethynyl)benzene (6).A 25 mL two-neck flask wascharged with 23 (113 mg,0.585 mmol) and 1,2,4,5-tetraiodobenzene(81 mg,0.139 mmol),evacuated,and filled with argon.Dry piperidine (15
英语翻译
1,2,4,5-Tetra((3-(4-pyridyl)ethynyl)bicyclo[1.1.1]pent-
1-ylethynyl)benzene (6).A 25 mL two-neck flask was
charged with 23 (113 mg,0.585 mmol) and 1,2,4,5-tetraiodobenzene
(81 mg,0.139 mmol),evacuated,and filled with argon.
Dry piperidine (15 mL) was added from a syringe,and the
solution was degassed by three freeze-pump-thaw cycles.
Then,Pd(PPh3)4 (17 mg,2.5 mol %) was added from a tip tube,
and the reaction mixture was stirred for 4 days at 55 °C.More
Pd(PPh3)4 (17 mg,2.5 mol %) was added from a tip tube,and
the reaction was continued for 4 more days.Then,NaOH/
EDTA (0.1 M in water,5 mL) was added,and the mixture was
stirred for 10 min.The phases were separated,and the
aqueous layer was extracted with toluene (3 \2 5 mL).The
organic layers were combined,and the solvents were evaporated
under reduced pressure.The crude product was dissolved
in chloroform and dried over Na2SO4 before the solvent was
evaporated under vacuum.The solid was chromatographed by
PTLC (alumina,chloroform),and 6 was obtained as small
needles after crystallization from chloroform:55 mg (47%);
mp 199 °C (dec); 1H NMR (CDCl3,500 MHz) ä 2.48 (s,24 H),
7.23 (dd,J ) 4.5 Hz,J ) 1.5 Hz,8 H),7.40 (s,2 H),8.52 (dd,
J ) 4.5 Hz,J ) 1.5 Hz,8 H); 13C {1H} NMR (CDCl3,124 MHz)
ä 30.71,31.11,59.02,77.95,77.98,92.75,93.77,125.10,125.74,
131.06,134.85,149.71; IR (KBr) 548,584,652,694,731,747,
818,856,899,992,1021,1038,1091,1120,1216,1241,1260,
1287,1369,1384,1405,1447,1487,1532,1571,1592,1629,
2227,2605,2852,2877,2915,2968,3048 cm-1; MS (FAB+/
NOBA) m/z 843 ([M + H]+); MS (ESI +) m/z (rel int) 843 ([M +
H]+,100).Anal.Calcd for C62H42N4:C,88.33; H,5.02; N,6.65.
Found:C,88.43; H,4.90; N,6.58.
英语翻译1,2,4,5-Tetra((3-(4-pyridyl)ethynyl)bicyclo[1.1.1]pent-1-ylethynyl)benzene (6).A 25 mL two-neck flask wascharged with 23 (113 mg,0.585 mmol) and 1,2,4,5-tetraiodobenzene(81 mg,0.139 mmol),evacuated,and filled with argon.Dry piperidine (15
1,2,4,5 -四( ( 3 - ( 4 -吡啶基)乙炔)双环[ 1.1.1 ]压抑
1 - ylethynyl )苯( 6 ) .25毫升双颈瓶是
被控犯有23条( 113毫克,0.585浓度)和1,2,4,5 - tetraiodobenzene
( 81毫克,0.139浓度) ,疏散,并充满氩气.
干哌啶( 15毫升)加入从注射器,和
解决办法是由三个脱气冻结泵冻融周期.
然后,钯(三苯基膦) 4 ( 17毫克,2.5摩尔% )增加了从冰山管,
和反应混合物被搅动了4天,55 °角更多
钯(三苯基膦) 4 ( 17毫克,2.5摩尔% )增加了从冰山管,和
反应持续了4天.然后,氢氧化钠/
乙二胺四乙酸( 0.1米的水,5毫升)加入,并混合了
搅拌10分钟.相分离,并
水层提取甲苯( 3 5毫升) .那个
有机层相结合,与溶剂的蒸发
根据减少的压力.原油产品被解散
在氯仿和干果超过硫酸钠之前溶剂
真空状态下蒸发.固体的是层析
PTLC (氧化铝,氯仿) ,并获得6小
针头后结晶从氯仿:55毫克( 47 % ) ;
熔点199 ℃ ( 12月) ;的1H NMR ( CDCl3 ,500兆赫)在2.48 (秒,24小时) ,
7月23日(日,强) 4.5赫兹,强) 1.5赫兹,8小时) ,7.40 (秒,2小时) ,8.52 (日,
J )条4.5赫兹,强) 1.5赫兹,8小时) ;的13C ) (质子核磁共振( CDCl3 ,124兆赫)
ä 30.71 ,31.11 ,59.02 ,77.95 ,77.98 ,92.75 ,93.77 ,125.10 ,125.74 ,
131.06 ,134.85 ,149.71 ;红外(溴化钾) 548 ,584 ,652 ,694 ,731 ,747 ,
818 ,856 ,899 ,992 ,1021年,1038年,1091年,1120年,1216年,1241年,1260年,
1287年,1369年,1384年,1405年,1447年,1487年,1532年,1571年,1592年,1629年,
2227年,2605年,2852年,2877年,2915年,2968年,三千零四十八厘米- 1 ;毫秒(轰击+ /
野场)米/ Z用843 ( [的M + H ]条+ ) ;毫秒(喷雾+ )米/环Z (相对国际) 843 ( [的M +
H ]条+ ,100 ) .肛门.Calcd为C62H42N4 :ć ,88.33 ;小时,5.02 ;氮,6.65 .
发现:ć ,88.43 ;小时,4.90 ;氮,6.58 .