英语翻译1-(2,2¢-Bipyrimidin-5-yl)ethynyl-3-ethynylbicyclo[1.1.1]-pentane (15).A flask was charged with 14 (1.0 g,4.22 mmol),evacuated,and put under argon.Freshly sublimed 9 (4.3 g,37.1 mmol) was washed into the flask with dry triethylamine(3
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英语翻译1-(2,2¢-Bipyrimidin-5-yl)ethynyl-3-ethynylbicyclo[1.1.1]-pentane (15).A flask was charged with 14 (1.0 g,4.22 mmol),evacuated,and put under argon.Freshly sublimed 9 (4.3 g,37.1 mmol) was washed into the flask with dry triethylamine(3
英语翻译
1-(2,2¢-Bipyrimidin-5-yl)ethynyl-3-ethynylbicyclo[1.1.1]-
pentane (15).A flask was charged with 14 (1.0 g,4.22 mmol),
evacuated,and put under argon.Freshly sublimed 9 (4.3 g,
37.1 mmol) was washed into the flask with dry triethylamine
(30 mL).The solution was degassed by three freeze-pumpthaw
cycles,and Pd(PPh3)4 (243 mg,0.21 mmol) was added
from a tip tube.The yellow reaction mixture was stirred and
refluxed for 10 days.A white solid precipitated.The triethylamine
was evaporated directly from the reaction mixture into
a liquid nitrogen cooled trap.Excess 9 was sublimed from the
crude product.The remaining solid was dissolved in benzene
and washed with 2 M NaOH (15 mL).The aqueous layer was
extracted with benzene (2 \2 15 mL),and the organic phases
were combined.After drying over Na2SO4 and evaporation of
the solvents under reduced pressure the product was chromatographed
by PTLC (alumina,chloroform) to yield 15 as a
white powder.After recrystallization from benzene small
colorless plates of 15 were obtained:0.827 g (72%); mp 178
°C (dec); 1H NMR (CDCl3,500 MHz) ä 2.09 (s,1 H),2.43 (s,6
H),7.39 (t,J ) 4.9 Hz,1 H),8.95 (s,2 H),8.98 (d,J ) 4.9 Hz,
2 H); 13C {1H} NMR (CDCl3,124 MHz) ä 30.33,58.75,68.57,
73.67,82.00,97.02,119.72,121.53,158.11,159.65,159.95,
161.88; IR (KBr) 407,732,531,561,640,652,746,768,814,
843,942,1128,1259,1370,1384,1410,1450,1519,1557,2224,
2874,2913,2965,2994,3299 cm-1; MS (EI+) m/z 272 (M,20),
271 (M - H,40),247 (M - C2H,10),193 (8),166 (20),139
(70),111 (30),97 (35),69 (70),57 (95),42 (100); MS (ESI+)
m/z (rel int) 295 ([M + Na]+,100),273 ([M + H]+,98); HRMS
calcd 271.0984 ([M - H]+),found 271.0976.Anal.Calcd for
C17H12N4:C,74.98; H,4.44.Found:C,75.26; H,4.67.
英语翻译1-(2,2¢-Bipyrimidin-5-yl)ethynyl-3-ethynylbicyclo[1.1.1]-pentane (15).A flask was charged with 14 (1.0 g,4.22 mmol),evacuated,and put under argon.Freshly sublimed 9 (4.3 g,37.1 mmol) was washed into the flask with dry triethylamine(3
1 - ( 2,2 ¢ - Bipyrimidin - 5 -基)乙炔- 3 - ethynylbicyclo [ 1.1.1 ] -
戊烷( 15 ) .一瓶被指控犯有14个( 1.0克,4.22浓度) ,
疏散,并根据氩.新鲜升华9 ( 4.3克,
37.1浓度)是洗到瓶干三乙胺
( 30毫升) .解决的办法是脱气三个冷冻pumpthaw
周期,和Pd (三苯基膦) 4 ( 243毫克,0.21浓度)增加
从冰山管.黄河是搅拌反应混合物和
回流为10天.白色固体沉淀.在三乙胺
被蒸发直接到反应混合物
液态氮冷却的陷阱.超过9升华从
原油产品.剩下的固体溶解在苯
和洗2男氢氧化钠( 15毫升) .水层
提取苯( 2 15毫升) ,与有机相
合并.干燥后的Na2SO4和蒸发
溶剂的压力下减少该产品层析
由PTLC (氧化铝,氯仿) ,收益率15日为
白色粉末.由苯重结晶后,小
无色板的有15人获得:0.827克( 72 % ) ;手机178
℃ ( 12月) ;的1H NMR ( CDCl3 ,500兆赫)在9月2日(秒,1 h )项,2.43 (秒,6
h )项,7.39 (吨,强) 4.9赫兹,1 h )项,8.95 (秒,2小时) ,8.98 (四,强) 4.9赫兹,
2小时) ;的13C ) (质子核磁共振( CDCl3 ,124兆赫)在30.33 ,58.75 ,68.57 ,
73.67 ,82.00 ,97.02 ,119.72 ,121.53 ,158.11 ,159.65 ,159.95 ,
161.88 ;红外(溴化钾) 407 ,732 ,531 ,561 ,640 ,652 ,746 ,768 ,814 ,
843 ,942 ,1128年,1259年,1370年,1384年,1410年,1450年,1519年,1557年,2224年,
2874年,2913年,2965年,2994年,3299 cm - 1处;质谱( EI数据库+ )米/ Z用272 (男,20岁) ,
271 (男-小时,40 ) ,247 (男- C2H ,10 ) ,193 ( 8 ) ,166 ( 20 ) ,139
( 70 ) ,111 ( 30 ) ,97 ( 35 ) ,69 ( 70 ) ,57 ( 95 ) ,42 ( 100 ) ;毫秒(喷雾+ )
米/环Z (相对诠释) 295 ( [的M +钠] + ,100 ) ,273 ( [的M + H ]条+ ,98 ) ;人力资源管理系统
calcd 271.0984 ( [男性- H ]条+ ) ,发现271.0976 .肛门.Calcd为
C17H12N4 :ć ,74.98 ;小时,4.44 .发现:ć ,75.26 ;小时,4.67 .