Norborna-diene → Binor-S

Norbornadiene (bicyclo[2.2.1]hepta-2,5-diene) was dimerized with the catalyst system CoBr2 -(triphenylphosphine)2 -boron trifluoride etherate. The structure of the diene is as follows: ##STR3## Afterwards methylene chloride was used to dissolve the organic phase of the reaction mixture and to separate the latter from the inorganic phase of catalyst components. Then the methylene chloride solution was washed with potassium carbonate to neutralize any free halogen acid and dried with the use of a drying agent such as anhydrous sodium sulfate. Upon cooling the treated methylene chloride solution Binor-S crystallized. The crystals were filtered from the liquid and then vacuum distilled to give solid Binor-S which had a grayish tinge. The foregoing procedure has been described in the literature. This procedure yields a Binor-S containing a trace amount of indigenous halide.

1. dissolutionto dissolve the organic phase of the reaction mixture
2. customto separate the latter from the inorganic phase of catalyst components
3. washThen the methylene chloride solution was washed with potassium carbonate
4. dry with materialdried with the use of a drying agent such as anhydrous sodium sulfate
5. temperatureUpon cooling the treated methylene chloride solution Binor-S
6. customcrystallized
7. filtrationThe crystals were filtered from the liquid
8. distillationvacuum distilled

ORD record

ord-33b65dd3b70e4838a15db2e9667867c4

Source dataset

uspto-grants-1977_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04064180