英语翻译1-(5¢-n-Hexyl-2,2¢-bipyridin-5-yl)ethynyl-3-ethynylbicyclo[1.1.1]pentane (22).A solution of 18 (520 mg,1.63mmol) in dry triethylamine (10 mL) under argon was transferredinto a 50 mL two-neck flask via cannula.Freshlysublimed 9 (
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英语翻译1-(5¢-n-Hexyl-2,2¢-bipyridin-5-yl)ethynyl-3-ethynylbicyclo[1.1.1]pentane (22).A solution of 18 (520 mg,1.63mmol) in dry triethylamine (10 mL) under argon was transferredinto a 50 mL two-neck flask via cannula.Freshlysublimed 9 (
英语翻译
1-(5¢-n-Hexyl-2,2¢-bipyridin-5-yl)ethynyl-3-ethynylbicyclo[
1.1.1]pentane (22).A solution of 18 (520 mg,1.63
mmol) in dry triethylamine (10 mL) under argon was transferred
into a 50 mL two-neck flask via cannula.Freshly
sublimed 9 (1.12 g,9.81 mmol) was rinsed into the flask with
dry triethylamine (15 mL),and the solution was degassed by
three freeze-pump-thaw cycles.Then,Pd(PPh3)4 (47 mg,2.5
mol %) was added from a tip tube.The reaction mixture was
heated to 70 °C for 15 h.The solvent was evaporated,and excess 9 was sublimed out under reduced pressure.The crude
product was dissolved in chloroform and washed with NaOH/
EDTA (0.1 M in water,2 \2 20 mL).The organic layer was
dried over Na2SO4,and the solvents were evaporated under
reduced pressure.The crude product was chromatographed by
PTLC (alumina/hexanes-ethyl acetate,15:1),and 22 was
obtained as a white powder:438 mg (76%); mp 146 °C; 1H
NMR (CDCl3,500 MHz) ä 0.85 (t,J ) 7.3 Hz,3 H),1.30 (m,6
H),1.59 (m,2 H),2.09 (s,1 H),2.41 (s,6 H),2.62 (t,J ) 7.7
Hz,2 H),7.58 (dd,J ) 8.1 Hz,J ) 1.8 Hz,1 H),7.75 (dd,J )
8.3 Hz,J ) 2.0 Hz,1 H),8.26 (d,J ) 8.4 Hz,1 H),8.29 (d,J
) 8.4 Hz,1 H),8.47 (d,J ) 1.6 Hz,1 H),8.66 (d,J ) 1.6 Hz,
1 H); 13C {1H} NMR (CDCl3,124 MHz) ä 14.03,22.52,28.75,
30.05,30.51,30.98,31.57,32.84,58.71,68.33,77.20,82.31,
91.98,119.45,119.90,120.92,136.76,138.56,139.54,149.41,
151.74,153.07,154.94; IR (KBr) 403,534,640,653,743,835,
928,1024,1050,1130,1224,1255,1272,1384,1465,1537,
1589,2854,2876,2926,2959,2992,3291 cm-1; MS (EI+) m/z
(rel int) 354 ([M]+,100),353 ([M - H]+,80),297 ([M - C4H9]+,
9),283 ([M - C5H11]+,95),268 (5),254 (12),241 (5),217 (13),
204 (6),190 (11),178 (5),163 (5),149 (7),115 (4),83 (4),69
(15),55 (14); HRMS calcd 354.2096,found 354.2089.Anal.
Calcd for C25H26N2:C,84.71; H,7.39; N,7.90.Found:C,84.64;
H,7.34; N,7.87.
英语翻译1-(5¢-n-Hexyl-2,2¢-bipyridin-5-yl)ethynyl-3-ethynylbicyclo[1.1.1]pentane (22).A solution of 18 (520 mg,1.63mmol) in dry triethylamine (10 mL) under argon was transferredinto a 50 mL two-neck flask via cannula.Freshlysublimed 9 (
1 - ( 5 ¢ - N -已基- 2 , 2 ¢ - bipyridin - 5 -基)乙炔- 3 - ethynylbicyclo [
1.1.1 ]戊烷( 22 ) .解决18个( 520毫克, 1.63
浓度)在干三乙胺( 10毫升)的氩气被移送
到50毫升两个颈部瓶通过套管.新鲜
升华9 ( 1.12克, 9.81浓度)是冲洗成瓶的
干三乙胺( 15毫升) ,以及解决办法是由脱气
三个冷冻泵冻融周期.然后,钯(三苯基膦) 4 ( 47毫克, 2.5
摩尔% )增加了从冰山管.是的反应混合物
加热到70 ° C 15小时该溶剂蒸发,和超过9升华下减少的压力.原油
产品被解散氯仿和洗涤用NaOH /
乙二胺四乙酸( 0.1米的水, 2 ? 20毫升) .有机层
干燥的硫酸钠和溶剂的蒸发下
减少压力.原油产品层析的
PTLC (氧化铝/ hexanes ,乙酸乙酯, 15时01分)和22
获得的白色粉末: 438毫克( 76 % ) ;熔点146 ℃ ;核磁共振
核磁共振( CDCl3 , 500兆赫)在0.85的( t , J )条7.3赫兹, 3小时) , 1月30日(男, 6
h )项, 1.59 (男, 2小时) , 2.09 (秒, 1 h )项, 2.41 (秒, 6小时) , 2.62 (吨,强) 7.7
赫兹, 2小时) , 7.58 (日,强) 8.1赫兹,强) 1.8赫兹, 1 h )项, 7.75 (日,强)
8.3赫兹,强) 2.0赫兹, 1 h )下, 8月26日(四,强) 8.4赫兹, 1 h )下, 8月29日(四,强
) 8.4赫兹, 1 h )项, 8.47 (四,强) 1.6赫兹, 1 h )项, 8.66 (四,强) 1.6赫兹,
1 h )段;碳) (氢核磁共振( CDCl3 , 124兆赫)在3月14日, 22.52 , 28.75 ,
5月30日, 30.51 , 30.98 , 31.57 , 32.84 , 58.71 , 68.33 , 77.20 , 82.31 ,
91.98 , 119.45 , 119.90 , 120.92 , 136.76 , 138.56 , 139.54 , 149.41 ,
151.74 , 153.07 , 154.94 ;红外(溴化钾) 403 , 534 , 640 , 653 , 743 , 835 ,
928 , 1024 , 1050 , 1130 , 1224年, 1255年, 1272年, 1384年, 1465年, 1537年,
1589年, 2854年, 2876年, 2926年, 2959年, 2992年, 3291厘米- 1 ;质谱( EI数据库+ )米/ ž
(相对诠释) 354 (模式[ M ] + , 100 ) , 353 ( [男性- H ]条+ , 80 ) , 297 ( [男性- C4H9 ] + ,
9 ) , 283 ( [男性- C5H11 ] + , 95 ) , 268 ( 5 ) , 254 ( 12 ) , 241 ( 5 ) , 217 ( 13 ) ,
204 ( 6 ) , 190 ( 11 ) , 178 ( 5 ) , 163 ( 5 ) , 149 ( 7 ) , 115 ( 4 ) , 83 ( 4 ) , 69
( 15 ) , 55 ( 14 ) ;高分辨calcd 354.2096 , 354.2089发现.肛门.
Calcd为C25H26N2 : ć , 84.71 ;小时, 7.39 ;氮, 7.90 .发现: ć , 84.64 ;
小时, 7.34 ;氮, 7.87 .
大夸张了,是不是应该发到别的地方,这里只怕是难以找到这样的人才。
一楼`
你牛.B ` 不知道是真的还是假的`
你没必要这么拼命吧``
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起码50`辛苦分
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