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).