Oxime formation problems...

[cublium]

This was cub's first oxime dream.He mixed 22 mls of water and 12 grams of anhydrous Na2CO3(prepared from NaHCO3).Result was a slurry.He added to this 13 grams of hydroxylamine hydrochloride(99% from Fluka).To this was added 25 grams of ketone dissolved in 110 mls of ethanol denat with 5-10% of IPA.This was refluxed with stirring in 1 liter roundbottom flask for an hour and a half.Added 100 mls of water and cooled in freezer,something oiled out.When mix was cold,upper layer was decanted and oil that was left was washed 3 times with water.Nothing seemed to crystallize.Oil smells same as ketone does(but seems to be lot more viscous) which made cub wonder if he had failed.What could be problem?Thanks

[cublium]

Cub noticed this slurry became thicker and thicker as it stood in freezer and now seems to be completely solid,sorry,cub was just impatient.Does this look like a healthy oxime(it's actually snow white,just pic was taken in not very brigth room)?

[cublium]

Cub screwed up reduction. He used 0,1 mm foil and reaction was very slow and didn't heat up.HgCl2 was added more than enough.Cub thinks he used too thick foil.How thick foil should be used?

[Rhodium]

0.025 mm foil is said to work great.

[Chromic]

Yeah, you should use thin aluminum foil... or the heavy duty foil, not the pie plate stuff. However, if all of the aluminum foil was turned into mush by the mercury/acetic acid, then you're good to go and you should be able to recover something from the post-rxn mixture.

[cublium]

Cub dreamed another 41 grams of oxime.Cub doesn't like these aluminium amalgamation,not at all.Anyways anhydrous ethanol and sodium metal are on the way,will post results should something arrive.

[Chromic]

AcOH/oxime/Hg/water/MeOH/Al worked fine for SWIC. Read the peracetic write up for details.

[cublium]

Hmmm...seems interesting.You added all aluminium at once?Used reynolds 0.025 mm?If cub gets his hands on some he will try this out.