busybird
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pyrrolidinyl-cyclohexyl-carbonitrile does not stay crystallize
126g of sodium bisulfite was dissolved in 420 mL of H2O. 106 g of cyclohexanone was added with vigorous stirring. The bisulfite adduct formed
immediately as a thick white slurry. The slurry was then cooled with an ice bath, and a solution of 78.6g KCN and 94.8 g pyrrolidine was added. After
stirring overnight at room temperature followed by cooling in an ice bath, the PCC did not crystallize. So stirred it vigorously and it did
crystallize but the crystals melt at room temp. So I let the crystals melt dissolved it with hexanes, dried with sodium sulfate, and evaporated the
solvent in a roto-vap but same as before.
I would just like to keep the crystals . Does anyone have any advice?
[Edited on 12-10-2014 by busybird]
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forgottenpassword
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I have a similar problem with my water crystals.
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skip
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I know this topic is quite old. I would like to add information for future reference. When pyrrolidine is used , no crystals form. Its a yellow, clear
oil isolated by extraction and not filtration. The final comp. is not even worth the cost or trouble.
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