tags
potassiumsodiumketonebisulfitesodium bisulfiteauxamDCMacetonemagnesium sulfatehydroxylamine

video tutorial Make potassium hydroxylamine disulfonate

Summary:

  • The video documents attempts to synthesize hydroxylamine via reduction of nitrite with bisulfite under strict cold conditions, aiming to form a sodium hydroxylamine disulfate salt.
  • Initial efforts tried converting the sodium salt to a potassium salt to encourage crystallization and attempted to form an auxiliary amine (auxam) by reacting with a ketone; distillation and extraction yielded little or no recoverable product.
  • Revisions on a smaller scale with careful temperature control achieved crystallization when converting to the potassium salt, yielding a significant amount of solid (potassium hypoxylamine disulfonate) upon purification, with an estimated dry yield around half to sixty percent.
  • The product could be oxidized to a distinct Fremi-salt, indicating a substantial amount of potassium hypoxylamine disulfonate and suggesting the intermediate could be of interest as an OTC precursor.
  • Conclusions advocated small-batch experiments, minimal water and ice, and favoring the potassium salt pathway over direct routes to hydroxylamine, with further updates planned.

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