The Vespiary

The Hive => Newbee Forum => Topic started by: cublium on October 07, 2003, 11:23:00 AM

Title: Oxime formation problems...
Post by: cublium on October 07, 2003, 11:23:00 AM: 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
Title: Sorry,false alarm...
Post by: cublium on October 07, 2003, 11:57:00 AM: 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)?
(https://www.thevespiary.org/rhodium/Rhodium/hive/hiveboard/picproxie_docs/000463227-file_s2si.jpg)
Title: failure in reduction
Post by: cublium on October 08, 2003, 07:34:00 AM: 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?
Title: foil thickness
Post by: Rhodium on October 09, 2003, 03:04:00 PM: 0.025 mm foil is said to work great.
Title: Use thin foil
Post by: Chromic on October 11, 2003, 09:52:00 AM: 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.
Title: Cub dreamed another 41 grams of oxime.Cub...
Post by: cublium on October 12, 2003, 12:10:00 PM: 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.
Title: AcOH/oxime/Hg/water/MeOH/Al worked fine for...
Post by: Chromic on October 13, 2003, 08:28:00 PM: AcOH/oxime/Hg/water/MeOH/Al worked fine for SWIC. Read the peracetic write up for details.
Title: Hmmm...seems interesting.You added all ...
Post by: cublium on October 13, 2003, 09:22:00 PM: 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.