I've recently been having some luck by dissolving the crude reaction mixture in diethyl ether (as concentrated as you can), layering on pentane and leaving the sealed flask overnight - by morning the oxide has mostly crystallised out. Comparatively low effort procedure :)
I've recently been having some luck by dissolving the crude reaction mixture in diethyl ether (as concentrated as you can), layering on pentane and leaving the sealed flask overnight - by morning the oxide has mostly crystallised out. Comparatively low effort procedure :)
Thank you Mr. Imre Tóth, Krassimira Guerra , Elisenda Reixach and John James Hayward for your valuable suggestion and feedback. I will work on the suggested methods.
Thank you Mr. Imre Tóth, Krassimira Guerra , Elisenda Reixach and John James Hayward for your valuable suggestion and feedback. I will work on the suggested methods.
I have performed several reactions where the byproduct is triphenylphosphine oxide. The simplest way I have found to get rid of PPh3O is to dissolve the reaction mixture in ethanol, add 2 equivalents of zinc chloride (2 equivalents in comparison to PPh3) and stir for a couple of hours at room temperature. This forms a PPh3O-Zn complex, insoluble in ethanol, and can be filtered off. Refer to this paper for more information: ArticleRemoval of Triphenylphosphine Oxide by Precipitation with Zi...
I have performed several reactions where the byproduct is triphenylphosphine oxide. The simplest way I have found to get rid of PPh3O is to dissolve the reaction mixture in ethanol, add 2 equivalents of zinc chloride (2 equivalents in comparison to PPh3) and stir for a couple of hours at room temperature. This forms a PPh3O-Zn complex, insoluble in ethanol, and can be filtered off. Refer to this paper for more information: ArticleRemoval of Triphenylphosphine Oxide by Precipitation with Zi...
Triphenylphosphine oxide is poorly soluble in hexane. First I'd try to crystallize it out from your crude product mixture from or by adding hexane. Cooling down in cold diethyl ether could also lead to crystallization. (TPPO is a good iniator for crystallization.) You can also try chromatography of crude products using etheral or hexane solutions. If nothing works you could also think about selective complex formation either with TPPO or with the diolefine. There are lots of TPPO complexes known (see attachment below). Of course, selectivity should be checked first in this case.
Triphenylphosphine oxide is poorly soluble in hexane. First I'd try to crystallize it out from your crude product mixture from or by adding hexane. Cooling down in cold diethyl ether could also lead to crystallization. (TPPO is a good iniator for crystallization.) You can also try chromatography of crude products using etheral or hexane solutions. If nothing works you could also think about selective complex formation either with TPPO or with the diolefine. There are lots of TPPO complexes known (see attachment below). Of course, selectivity should be checked first in this case.
The synthesis of NiCl2(OPPh3)2 was among the references I've sent above.
The synthesis of NiCl2(OPPh3)2 was among the references I've sent above.
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I've recently been having some luck by dissolving the crude reaction mixture in diethyl ether (as concentrated as you can), layering on pentane and leaving the sealed flask overnight - by morning the oxide has mostly crystallised out. Comparatively low effort procedure :)
I've recently been having some luck by dissolving the crude reaction mixture in diethyl ether (as concentrated as you can), layering on pentane and leaving the sealed flask overnight - by morning the oxide has mostly crystallised out. Comparatively low effort procedure :)
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VOTE
Thank you Mr. Imre Tóth, Krassimira Guerra , Elisenda Reixach and John James Hayward for your valuable suggestion and feedback. I will work on the suggested methods.
Thank you Mr. Imre Tóth, Krassimira Guerra , Elisenda Reixach and John James Hayward for your valuable suggestion and feedback. I will work on the suggested methods.
More
VOTE
I have performed several reactions where the byproduct is triphenylphosphine oxide. The simplest way I have found to get rid of PPh3O is to dissolve the reaction mixture in ethanol, add 2 equivalents of zinc chloride (2 equivalents in comparison to PPh3) and stir for a couple of hours at room temperature. This forms a PPh3O-Zn complex, insoluble in ethanol, and can be filtered off. Refer to this paper for more information: Article Removal of Triphenylphosphine Oxide by Precipitation with Zi...
I have performed several reactions where the byproduct is triphenylphosphine oxide. The simplest way I have found to get rid of PPh3O is to dissolve the reaction mixture in ethanol, add 2 equivalents of zinc chloride (2 equivalents in comparison to PPh3) and stir for a couple of hours at room temperature. This forms a PPh3O-Zn complex, insoluble in ethanol, and can be filtered off. Refer to this paper for more information: Article Removal of Triphenylphosphine Oxide by Precipitation with Zi...
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Triphenylphosphine oxide is not soluble at all in pentane. You could try chromatography the crude of the reaction with this solvent.
Triphenylphosphine oxide is not soluble at all in pentane. You could try chromatography the crude of the reaction with this solvent.
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Triphenylphosphine oxide is poorly soluble in hexane. First I'd try to crystallize it out from your crude product mixture from or by adding hexane. Cooling down in cold diethyl ether could also lead to crystallization. (TPPO is a good iniator for crystallization.) You can also try chromatography of crude products using etheral or hexane solutions. If nothing works you could also think about selective complex formation either with TPPO or with the diolefine. There are lots of TPPO complexes known (see attachment below). Of course, selectivity should be checked first in this case.
Triphenylphosphine oxide is poorly soluble in hexane. First I'd try to crystallize it out from your crude product mixture from or by adding hexane. Cooling down in cold diethyl ether could also lead to crystallization. (TPPO is a good iniator for crystallization.) You can also try chromatography of crude products using etheral or hexane solutions. If nothing works you could also think about selective complex formation either with TPPO or with the diolefine. There are lots of TPPO complexes known (see attachment below). Of course, selectivity should be checked first in this case.
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If your compound doesn’t coordinate with Ni you can explore de the tetrahedral species NiCl2(OPPh3and try to crystallize it to remove
If your compound doesn’t coordinate with Ni you can explore de the tetrahedral species NiCl2(OPPh3and try to crystallize it to remove
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