well ive been realy interested in making esters of
cinnamic acid derivatives and thanks to some resurch
done by two very kind bee's (you know who you are
and thankyou I love you guys )
ive been able to make some butyl and ethyl esters
of alpha methyl .
well there was a lot of hype about this synth for a wial.
but I think most people are not into perfume so I guess
it fizzeled out.
so about the tests.
as stated by thouse two bee's and a few patents it
is not worth going by aquas condensation.
well this is not realy true.
infact its damb wrong aquas rocks.
solvents dont make any effect on the reaction if
done in aquas conditions.
things like ethanol and glycerol can be in the reaction.
yep you dont quite get the yeilds of an anhydrous
reaction. But in defence of the aquas reaction the
butenone will crystalize out of the solution after
5 to 10 days all on its own.
I also belive due to the higher ph and longer reaction
time that you get less to no polymer product.
I was told this could be done on piperonal as well.
I dont think this is true as anything attatched to the
benzene ring at possition 3 will induce a dual condensation.
ie you will end up with a dibenzyl product one ring on each
side of the ketal group.
I havent tried this (I do hope it works as I love the
smell of that methylene dioxy and would love to
smell the esters of its acids.) and it may actualy be possible
as the ether on 3 is joined to 4. but I think if it did work
yeild would be low.
well after aldol there was some resurch done on the haloform.
I found it very difficult to seperate the acid from solution
by traditional methods.
But if one filters then turns solution acidic then adds caustic
till no more preciptate falls out it gets realy easy.
once precipitate has been collected just add a small amount
of acid to convert the salt back into its acid and you get
clear platellets of alpha methyl
no solvent extraction no heat.
oh somthing I forgot to mention in classic documentation
they use too little acid in the aquas reaction.
I think the more the better as you have the water as
a buffer to stop polymerization.
I have found little to no technical documentation on
alpha methyl acids and im having to go by my nose most
of the time. If any one has some real data on these
compounds please let me know. I have melting point and
boiling point ect what I need is its solubilities and the
solubilities of its salts.
and a word of warning when I isolated the acids salt
I nearly shat my self, I had to run to the toilet and
stayed there for quite some time. not pleasant. dont
smell the salt, I dont think its the salt but
rather an impurity left from the haloform.
hope I have helped and thanks guys my house dosnt
smell like dog piss anymore (should have given him the snip)
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