Saturday, March 28, 2009

Preparation of Cyclopentadiene

From: http://www.tcieurope.eu/en/product/synthetic-chem/S026.shtml

The reaction apparatus (Figure 1) is assembled by attaching a thermometer, Vigreaux distilling column and Liebig condenser to a 500ml two necked flask. The receiver is cooled by means of a refrigerants or freezing mixtures.
Dicyclopentadiene (195g) is placed in the two necked flask and heated to about 160ºC with an electric heating mantle or oil bath. Thermal decomposition begins at about 150ºC and distillates at 43 ~ 46ºC can be obtained (addition of iron powder expedites the thermal decomposition rate of Cyclopentadiene). Heating is applied slowly, because rapid temperature increases cause dicyclopentadiene to distill prior to undergoing thermal decomposition. In such a case, re-distillation allows narrow boiling-point distillates.
Cyclopentadiene dimerzes rapidly at room temperature and should be used immediately.

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