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PMK synth
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valmont

Joined: 08 Sep 2005
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Thu Sep 08, 2005 7:16 am
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SWIM came across a product in china that was unreleased with no CAS number which was an intermediate for piperonyl methyl ketone. Apparently it was a solid and their was a certain procedure u need to do with costic soda and HCL acid to give u 99.9% transparent PMK.

has anyone even heard of such a thing? i think an underground chemist had invented it. the intermediate had epoxypropinate in the title from what SWIM can remember. Question
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joe_aldehyde
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Joined: 06 Apr 2005
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Thu Sep 08, 2005 1:59 pm
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it probably was the bisulfite adduct or the sodium iodide adduct. could also have been the epoxide, but there is no such thing as an epoxypropinate.
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fcknut

Joined: 19 Apr 2005
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Thu Sep 08, 2005 8:30 pm
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joe_aldehyde wrote:
but there is no such thing as an epoxypropinate.


epoxypropionate maybe...?
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valmont

Joined: 08 Sep 2005
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Fri Sep 09, 2005 2:43 pm
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yes, it was epoxypropionate with 3-4 MDP methyl b4 it i think.... but it was an intermediate that could not be found anywhere else. im assuming this underground chemist had made it, so my question is if anyone had heard of such a thing and/or why havnt others tried to patent such intermediates for PMK
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joe_aldehyde
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Fri Sep 09, 2005 4:22 pm
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i don't see how one would go from an epoxide acid to a ketone. hydrolysis of the epoxide occurs first, giving a glycol or an alcohol, by dehydration giving a benzylic ketone or an a,b-unsaturated acid (ester).
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Lego

Joined: 15 Apr 2005
Posts: 52
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Fri Sep 09, 2005 5:39 pm
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Under anhydrous conditions no hydrolysis will occur.
Epoxides are isomeric to ketones
Additon of a lewis acid opens the epoxide and will give a stabilised benzylic cation which rearranges to the ketone. Plenty of examples in text books....
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joe_aldehyde
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Fri Sep 09, 2005 6:44 pm
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well, lego - to a benzylic ketone, therefor useless. and with the carboxylate or ester group, thats still another story.
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Lego

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Fri Sep 09, 2005 7:37 pm
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joe_aldehyde wrote:
well, lego - to a benzylic ketone, therefor useless. and with the carboxylate or ester group, thats still another story.


No, the benzylic cation is stabilised, therefore the benyzl-methyl-keton (aka P2P) will form. The oxygen will stick to carbon next to benzylic carbon, because otherwise a secondary cation will be the intermediate which is less stable than the benzylic one.

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joe_aldehyde
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Fri Sep 09, 2005 10:36 pm
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i can very well see your point (excuse me, i'm just a novice in OC) - i always thought that the most conjugated series of double bonds is responsible for the selectivity towards the product - thats the case for the benzylic ketone.
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valmont

Joined: 08 Sep 2005
Posts: 5
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Sat Sep 10, 2005 5:50 am
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so im guessing the intermediate title wasnt correct then? what i never understood was how they came about making the intermediate for the Pmk
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joe_aldehyde
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Sat Sep 10, 2005 1:34 pm
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why don't you go about finding out what the real intermediate compound name was, valmont?
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valmont

Joined: 08 Sep 2005
Posts: 5
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Sun Sep 11, 2005 2:08 pm
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3,4 (methlenedioxy phenyl) methyl epoxypropionate.. i think but anyway could something be made possibly?? as in an intermediate for PMK
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joe_aldehyde
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Mon Sep 12, 2005 1:29 am
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from what i know, it is not a suitable intermediate for PMK.
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valmont

Joined: 08 Sep 2005
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Mon Sep 12, 2005 7:33 am
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thanks joe Smile

any thoughts on what is a suitable or the most suitable intermediate for PMK?

it would be much appreciated thanks
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joe_aldehyde
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Mon Sep 12, 2005 4:19 pm
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go have a look at the hive files...intermediates are mostly made from watched precursors. i don't know of any intermediates that are commercially available and unwatched.
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