http://www.erowid.org/archive/rhodium/chemistry/eleusis/bisulfite.html
while reading this a few questions came to mind.....and was wondering
1) does this make it were your ketone would not have to be distilled, thus making one only have to distill the sass.
2)or could this be a step to purify it, by taking ketone turning it into the crystalline, then when ready to use extract it and distill it.
3)or should it be distilled first then done?
4) is this just meant to be a way to store the ketone?
The last thing is help with the moles..
1) Preparation of the bisulfite reagent
(This must be prepared just prior to use, as it will autooxidize within hours if left to it's own devices.)
Add 52g sodium bisulfite (NaHSO3, .5moles) to approximately 90mL of distilled water at room temperature with vigorous stirring (slightly more water may be used to get it all into solution). Add a volume of denatured alcohol of about 70% of the solution's volume (ie - if you end up with 100mL of solution, add 70mL of alcohol) then add more water to just dissolve the precipitate (~60mL).
2) Reacting with the ketone
Slowly drip .25moles of ketone(*) into a beaker containing the bisulfite solution with vigorous magnetic stirring. The 2:1 molar ratio insures that all of the ketone will be converted. Let sit on the stirrer for an additional 30-45 minutes then filter on a vacuum Buchner funnel. Wash the crystals with 20-50mL of denatured alcohol. Dry in a vacuum dessicator or open tray then store in a stoppered glass bottle until needed.
(*) If adding an impure reaction matrix, add as much solution as you expect to contain .25moles of ketone.
3) Recovering the ketone
Add the ~.25moles of bisulfite addition product to a separatory funnel then slowly pour in 105mL of 10% Sodium Hydroxide solution (w/w). Separate out the aqueous layer (which may be on top or on bottom depending on the ketone), saturate with salt (NaCl), and extract with 50mL of ether (toluene or benzene ok if the ketone is of high enough bp). Combine the extract with the ketone layer and strip off the ketone by distillation (condense and reuse!). Distill the ketone residue, preferably under vacuum (if you're making what I think you're making), to yield up to 90%, depending on the purity of the starting ketone, of course.
What exactly would be .25 moles of ketone
and what would be .25 moles of ketone bisulfite?
Your help would be great, as well as experiences with this!
while reading this a few questions came to mind.....and was wondering
1) does this make it were your ketone would not have to be distilled, thus making one only have to distill the sass.
2)or could this be a step to purify it, by taking ketone turning it into the crystalline, then when ready to use extract it and distill it.
3)or should it be distilled first then done?
4) is this just meant to be a way to store the ketone?
The last thing is help with the moles..
1) Preparation of the bisulfite reagent
(This must be prepared just prior to use, as it will autooxidize within hours if left to it's own devices.)
Add 52g sodium bisulfite (NaHSO3, .5moles) to approximately 90mL of distilled water at room temperature with vigorous stirring (slightly more water may be used to get it all into solution). Add a volume of denatured alcohol of about 70% of the solution's volume (ie - if you end up with 100mL of solution, add 70mL of alcohol) then add more water to just dissolve the precipitate (~60mL).
2) Reacting with the ketone
Slowly drip .25moles of ketone(*) into a beaker containing the bisulfite solution with vigorous magnetic stirring. The 2:1 molar ratio insures that all of the ketone will be converted. Let sit on the stirrer for an additional 30-45 minutes then filter on a vacuum Buchner funnel. Wash the crystals with 20-50mL of denatured alcohol. Dry in a vacuum dessicator or open tray then store in a stoppered glass bottle until needed.
(*) If adding an impure reaction matrix, add as much solution as you expect to contain .25moles of ketone.
3) Recovering the ketone
Add the ~.25moles of bisulfite addition product to a separatory funnel then slowly pour in 105mL of 10% Sodium Hydroxide solution (w/w). Separate out the aqueous layer (which may be on top or on bottom depending on the ketone), saturate with salt (NaCl), and extract with 50mL of ether (toluene or benzene ok if the ketone is of high enough bp). Combine the extract with the ketone layer and strip off the ketone by distillation (condense and reuse!). Distill the ketone residue, preferably under vacuum (if you're making what I think you're making), to yield up to 90%, depending on the purity of the starting ketone, of course.
What exactly would be .25 moles of ketone
and what would be .25 moles of ketone bisulfite?
Your help would be great, as well as experiences with this!
