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DraconicAcid
International Hazard
Posts: 4278
Registered: 1-2-2013
Location: The tiniest college campus ever....
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Mood: Semi-victorious.
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Quote: Originally posted by blogfast25  |
The solvent was acetonitrile:acetic acid (3:2), not for everyone, that. Reported yields were generally good. Wonder if this works also with the
straight alcohols. Or perhaps using acetone as a solvent?
Interesting find. |
You need the acetic acid there to make the solution acidic. If you wanted to make it easier to isolate the organic product, you could probably use an
inorganic acid such as phosphoric, I guess. Just not as much.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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gdflp
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Location: NY, USA
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Here is the procedure from my notebook :
38.66g of Ca(OCl)2(81.22g were used because the package listed it as 47.6%) was dissolved in 400ml of distilled water and the solution was
filtered to remove any insoluble salts which were present in the pool-grade chemical used. This was chilled to 0°C in an ice bath and strong
stirring was started. Next, a mixture of 50ml of glacial acetic and 19.4ml of benzyl alcohol was added dropwise via a separatory funnel. Finally,
the solution was allowed to warm to room temperature over a period of ten minutes while still stirring. The bottom layer of crude benzaldehyde was
removed using the separatory funnel to yield approximately 17ml of crude benzaldehyde as a slightly yellow oily liquid. No attempt was made to purify
the benzaldehyde as I do not have an apparatus small enough for distilling it and I didn't have any metabisulfite at the time.
I plan to revisit this synthesis soon and do various small scale tests utilizing different amounts of acetic acid as there was likely a large excess
of acetic acid, I just used a direct scaleup from the rhodium archive. Unfortunately, I don't have the funds at the moment to purchase any more
benzyl alcohol, so I will just ration the amount I have left.
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