process for the production of exo tetrahydrodicyclopentadien by hydrogenation of endo - dicyclopentadien and subsequent isomerisation of the endo - tetrahydrodicyclopentadiens

摘要

Prepn. of oxo-tetrahydrodicyclopentadiene (I) is carried out by (a) hydrogenating endo-dicyclopentadiene (II) contg. a dispersed Ni catalyst to form crude endo-tetrahydrodicyclopentadiene (III) with a m.pt. of at least 70 deg.C; (b) contacting the crude (III) with AlCl3 at 100-150 deg.C; and (c) sepg. the liq. phase comprising from the sludge phase of the reaction mixt. Hydrogenation is pref. effected in 2 stages: (1) at 110-120 deg.C to effect hydrogenation of the 8 and 9 positions; (2) at 150-200 deg.C to complete the hydrogenation. Step (b) is pref. effected in the presence of an inert solvent, esp. added (I). The AlCl3- rich sludge from step (c) is pref. recycled to step (b). (I) is a high-energy fuel for use in jet engeins, e.g. in missiles. The presence of spent Ni catalyst in the crude (III) ensures high conversions in step (b) with high selectivity for (I); e.g. 81-99% yields can be obtd.