英语翻译1,3-Di(1-chlorovinyl)bicyclo[1.1.1]pentane (12).37 A mixtureof 11 (1.82 g,0.012 mol),hexachloroethane (5.66 g,0.024mol),and triphenylphosphine (6.27 g,0.025 mol) was slowlyheated to 100 °C under stirring.After 1 h,the reaction flaskwas a
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英语翻译1,3-Di(1-chlorovinyl)bicyclo[1.1.1]pentane (12).37 A mixtureof 11 (1.82 g,0.012 mol),hexachloroethane (5.66 g,0.024mol),and triphenylphosphine (6.27 g,0.025 mol) was slowlyheated to 100 °C under stirring.After 1 h,the reaction flaskwas a
英语翻译
1,3-Di(1-chlorovinyl)bicyclo[1.1.1]pentane (12).37 A mixture
of 11 (1.82 g,0.012 mol),hexachloroethane (5.66 g,0.024
mol),and triphenylphosphine (6.27 g,0.025 mol) was slowly
heated to 100 °C under stirring.After 1 h,the reaction flask
was attached to a Kugelrohr apparatus,and the reaction mixture was distilled under vacuum (0.5 Torr) with one
receiving flask kept at room temperature,the second one
cooled to 0 °C with ice,and a third one cooled to -78 °C with
dry ice.The temperature in the oven was slowly raised to 120
°C,and the distillation was continued until only solids
remained in the distillation flask.After cooling to room
temperature,the first receiving flask was moved into the
Kugelrohr oven.The distillation was resumed and the oven
temperature slowly raised back to 120 °C.In the ice-cooled
flask,1.89 g (83%) of 12 was collected in a 20:1 mixture with
13.The second flask contained mostly tetrachloroethylene but
should always be checked for product.1H NMR (CDCl3,300
MHz) ä 2.04 (s,6 H),5.15 (d,2 H,J ) 1.5 Hz),5.20 (d,2 H,J
) 1.5 Hz).37 For 13:1H NMR (CDCl3,300 MHz) ä 1.99 (s,6
H),2.06 (s,3 H),5.17 (d,1 H,J ) 1.5 Hz),5.23 (d,1 H,J )
1.5 Hz).
英语翻译1,3-Di(1-chlorovinyl)bicyclo[1.1.1]pentane (12).37 A mixtureof 11 (1.82 g,0.012 mol),hexachloroethane (5.66 g,0.024mol),and triphenylphosphine (6.27 g,0.025 mol) was slowlyheated to 100 °C under stirring.After 1 h,the reaction flaskwas a
1-chlorovinyl)bicyclo叔[1.1.1]比较(12).37混合物
11(1.82 g 0.012组分),hexachloroethane(566 g 0.024)
组分)、四水合氯化亚铁与g 0.025组分(6.27)正在缓慢
加热到100℃下搅拌.一小时之后,人们的反应
被连接到一个Kugelrohr仪、反应蒸馏而来的是在真空环境下(0.5陶尔)和一个吗
在室温下接受瓶保存,第二个
冷却到0度了冰,第三个冷却到-78°C
乾冰.箱内温度缓慢上升到120华氏度
°C,蒸馏是一直持续到只有固体
住在蒸馏瓶.冷却后到另一个房间
温度,第一个接受瓶被搬进了
Kugelrohr烤箱.蒸馏后的恢复和烤箱里
温度慢慢提高回到120℃.在相关
瓶、1.89克(83%)12被收录在《20:1混合
13.第二个瓶含主要四氯乙烯但
应该检查产品.核磁共振(CDCl3,300名吗
兆赫)(6小时,2.04),2小时5.15(d)150赫兹),[J],(d、2小时
150赫兹).37)为十三核磁共振(CDCl3 300兆赫),(s、6、7、8 1.99
(H),2.06,3小时),5.17(d,1小时,J)150赫兹(d),1小时5.23,J).
150赫兹).