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Heck coupling protocols on the basis of Pd(OAc)2 and phosphane ligands as triphenylphosphane, other trisarylphosphanes as tris-o-tolylphosphane and tris-n-butylphosphane with different solvent systems and bases were investigated.
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Heck coupling protocols on the basis of Pd(OAc)2 and phosphane ligands as triphenylphosphane, other trisarylphosphanes as tris-o-tolylphosphane and tris-n-butylphosphane with different solvent systems and bases were investigated.
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2O. Yet, under these same conditions, the methyl ether derivative 17c was converted into the desired bromoenol triflate 10c without observing significant amounts of the non-desired regioisomer.
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2O. Yet, under these same conditions, the methyl ether derivative 17c was converted into the desired bromoenol triflate 10c without observing significant amounts of the non-desired regioisomer.
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1H NOESY experiments in which interactions within the steroid analogue cis-13b between the protons of the methyl group at C-13 and the proton at C-14 as well as between the proton at C-14 with the proton at C-7 were detected. Within the steroid trans-24b interactions between the methyl group at C-13 and the proton at C-8 could be observed and also interactions between the proton at C-7 with the proton at C-8 and the proton at C-14 with one proton at C-15 were found.
-
1H NOESY experiments in which interactions within the steroid analogue cis-13b between the protons of the methyl group at C-13 and the proton at C-14 as well as between the proton at C-14 with the proton at C-7 were detected. Within the steroid trans-24b interactions between the methyl group at C-13 and the proton at C-8 could be observed and also interactions between the proton at C-7 with the proton at C-8 and the proton at C-14 with one proton at C-15 were found.
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CCDC-618817 (trans-27) contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/ data_request/cif/
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CCDC-618817 (trans-27) contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/ data_request/cif/
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CCDC-618818 (33) contains the supplementary Crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif/
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CCDC-618818 (33) contains the supplementary Crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif/
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CCDC-618819 (37) contains the supplementary Crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam. ac.uk/data_request/cif/
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CCDC-618819 (37) contains the supplementary Crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam. ac.uk/data_request/cif/
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The methyl ester analogue of compound trans-27 was obtained along the same synthetic pathway, using the less cleanly and efficiently reacting methyl acrylate instead of tert-butyl acrylate in the Heck reaction.
-
The methyl ester analogue of compound trans-27 was obtained along the same synthetic pathway, using the less cleanly and efficiently reacting methyl acrylate instead of tert-butyl acrylate in the Heck reaction.
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