triphenylphosphineoxide
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Stone Age tecnology to Heterocyclic Synthesis in one lifetime.
Firstly a massive thank you to all who contribute here, this site is fantastic.
I realise that there are many threads here that deal with parts of my current experiment, but I am wondering if any one else has tried this or has any
suggestions.
My experiment is this; to advance as far as possible using knowledge and materials that I can grow or mine. I am starting using Stone Age techniques
no glassware, no controlled heating, nothing.
Currently I am processing ash to produce K2C03 and CaO using courboulli (boiled leather) vessels. Oxidising Manure under basic conditions to produce
Ca(NO2)3. Brewing via wild fermentation. Collecting bees wax and plant oils and mining clay and burning charcoal.
Anyone have a suggestion on what should come next, I am still a long way from smelting FeS and collecting SO3, so no novel oxazines are being made
any time soon.
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chromium
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I to not understand what exactly you want to achieve but there are some ideas you could use to make common chemicals with very simple means.
It should not be hard to make clay retort. If you have retort then you can pyrolyse organic material and make simple distillations.
If coal is pyrolysed in retort one gets complex mixture of organic compunds which contains benzene, toluene, xylenes, phenol anthrachene and others.
Some or all of these can be separated with quite acceptable purity if fractionated or just redistilled several times from retort. Of course you need
to use lot of coal for this.
If you use wood instead of coal you will get methanol, acetic acid and wood tar creosote that is mix of various phenolic compounds.
Acetic acid (you can make this by fermentation as well) can be converted to calcium acetate and this pyrolysed to acetone (using retort). Acetone
could be condensed to mesitylene (so you got benzene ring) or IIRC it can be partially converted to benzene if vapour is passed through tube on red
heat.
Alternatively you may find some plant that contains oxalic acid in free form (not as salt). Solution of oxalic acid decomposes NaCl to HCl and NaNO3
to HNO3 if strongly heated.
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Sandmeyer
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| Quote: | | I am starting using Stone Age techniques no glassware, no controlled heating, nothing. |
As far as organic sytnthesis goes you can go a long way with only beakers, filtering setup and vacuum source as equipment. When something calls for a
reflux it often isn't a requirement for the reaction to take place at the B.P temperature of the solvent, gentle heating is sufficient, or when it is
a requirement the rxn mix can be boiled in beaker and solvent added from time to time as it evaporates (preferably outside). Metallo-organic chemistry
and other "special" branches require a bit more sophisticated equipment, but one wants to avoid those methods as fas as possible even in a
well-equipped lab.
For those that can obtain some lab equippment but like me hate distillation then chromatography might be preferable for purification
of oils (in rare cases when they can't be purified by acid-base extraction, bisulfite complexing and simillar). A really conveniant method for up to
15 g material is dry-flash chromatography, which is as far as equimpent goes just like vacuum filtration but with a sinter funnel packed with silica
instad of a Büchner, only downside for the hobby chemist is to get silica and TLC plates...
[Edited on 3-8-2006 by Sandmeyer]
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triphenylphosphineoxide
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I am not hoping to achieve anything, I am interested in seeing how far I can go.
Motivation for this came from 8 days without power or gas thanks to storm damage.
In half an hour using materials salvaged from the recycling bin I had functioning oil lamps, and hot plate on which sat a very crude and leaky
still(there is still a scorch mark on the ceiling) converting my homebrew into fuel. When the glass in the lamps(coffee jars) cracked I turned all
suvivalist and made some fire hardened clay lamps.
Other motivating factors are the desire to leave no purchasing records and a vague feeling of impending societal collapse.
thankyou for the suggestions; acetone production will commence when I collect the Calcium salts, Oxalis and sourghum are now allowed to grow in my
garden, they should have extractable quantities of oxalic acid.
Hmm Vacuum source I may have to cheat a bit there, will try not to. Should be able to make bellows and crude one way valve. Still haven't made metal
tools, Clay blast furnace???
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Chris The Great
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Acetic acid from pyrolysing wood?? Do you have any more details for that? Because I am simply to cheap to buy GAA when I have huge piles of wood. I
am also interested in the capability to continue chemistry when society falls into a huge pile of smoking ruins, and methanol and AA would be useful
towards that end.
I take it you are making all of your equipment as well? Well, that's a bit further than I'd take it, I'd stick to my pieces of plastic hose from the
side of the road, old copper tubing from the dump and glass jars from my purchased food products (and also the side of the road).
Well good luck on the project! It sounds very interesting, although personally I think you'll be spending a lot of time just making simple pieces of
equipment.
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not_important
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If you've running water you may want to investigate hydralic ram pumps. Among other things they can be used to pump water from a source with a low
head, up to a decent elevation to get a water source with decent pressure. Once you've that, then consider aspirators for vacuum.
As for oxalic acid, a decent source is fusing sawdust with lye or potash in thin layers. For some detailed references :
http://pubs3.acs.org/acs/journals/doilookup?in_doi=10.1021/i...
http://pubs3.acs.org/acs/journals/doilookup?in_doi=10.1021/i...
http://pubs3.acs.org/acs/journals/doilookup?in_doi=10.1021/i...
About 3/4 of the wood ends up as oxalic, 18% as acetic, a few percent as formic. Caustic recovery can be 50 to 90%. I think you may be able to recover
some methanol from the gases released.
and using fungus :
http://aem.asm.org/cgi/reprint/11/3/255
http://aem.asm.org/cgi/content/abstract/13/5/732
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Marvin
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I certainly second the oxalic acid from sawdust rather than from plants, but the method needs sulphuric acid and a long purification process IIRC.
You will need to scale up to industrial quantities to get anywhere.
Formic acid is probably best made from oxalic acid.
Acetic acid is probably best made from ethanol.
Methanol from wood spirits, unless you plan to cut down and distill a small forest may not be feasable.
I suggest you break one part of the stone age process though - the dying early part.
Get some good protective gear, resperator, dust masks, etc. Organise where you do this to vent fumes.
Buy some clean sand and sodium carbonate and try making some glass. Victorian chemists mostly had to make all their own glassware. A charcoal
furnace may be clean enough.
Smelting copper ore is fairly trivial with the charcoal and bellows method. Iron from iron ore rather more difficult.
You will have to break some rules, noone has access to enough of the planets surface by walking to start a chemical industry.
Sulphuric acid by the bell jar process from sulphur/saltpeter.
A lot to try.
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not_important
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The standard sawdust oxalate purification was
- leaching the reaction mix with a small amount of cold water (sodium oxalate is sparingly soluble) to remove the caustic
- dissolve the sodium oxalate in hot water, filter
- add calcium hydroxide to the filtrate, cool, filter to collect calcium oxalate
- decompose that with fairly dilute sulfuric acid, filter
- concentrate filtrate to obtain oxalic acid.
.
The calcium salt sulfuric acid steps are part of most methods of isolating oxalic acid. Tying up sulfur as calcium sulfate is a downside to the
process.
A small scale alternative is to take the filtered sodium oxalate, concentrate it, take the crystallised oxalate, suspend in ethanol, treat with HCl
gas to ppt NaCl, let sit to form diethyl oxalate, wash with water. The ester can be distilled under reduced pressure for higher purity. Add a slight
excess of acetic acid to the ester, fractionate to remove ethyl acetate, a useful byproduct, leaving oxalic acid.
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