pars.lea.oil-brommyristic-european workinprogress

[cavos]

-i decided to try the reflux.
I refluxed it and then i added the hcl.Ammonium cloride formed and discarded.I cristallised yellow needls, i trayed approx 30 mg, it´s  smell like salt with a littlebit bitter aroma and the flavour is like gummy.
I decid to wash the product with 10% naoh in  dH2O.I save the organic layer and dry it.It´s come back the same oil colored like the pink floyd wall 1 ml. .fuck delepine.
Next try will be dillapiole in hbr and reflux or bomb with methilamine  and parallel dillapiole+koh and reduction with something.
ciao
cavos

[hypo]

you really should start to clean your intermediate products. we
have no idea why this failed: we don't even know whether you
really had myristicin (maybe the impurities crystallised on freezing!),
to start with!

if you really got an amine (you did an A/B, right) and used the
impurities in the oil, then god nows what you've got.

> or bomb with methilamine

that will give the N-methyl derivate, which is afaik more or less inactive.

[cavos]

I got foundamental 2 problem:
the first one
no magnetic stirrer
the second one
no fraction dist. column.
This year quarter I buyed a elettric plate and finally puted my old butan-propan camping plate in pension.
The next quarter I will buy a frac.dist.col.
My next step is following  parallel game:
distillation of nabr to become hbr,hbr gasing hbr with phosph.acid,finkelstein swap (or alternat.gas  ala judexk with nai red phosp) and
methylamine bomb.
isomerisation, peracid oxidation,and reduction with al/hg.
-you and the other old beeangels could help me in the following problem:
where can I find o.t.c.  in the good old  pacifist socialdemocratic europe DCM and PTC (De,At)?
Nec recida recedi.

[hypo]

> no magnetic stirrer

that sucks. you will have to work with overhead stirring.
but used magnetic stirrers can be had pretty cheap.

> no fraction dist. column.

before you buy a fractionating column: be sure to buy a vacuum pump.
that's much more important.

a column can be had for $10-$20. you don't need a fancy vigreux thing,
go with a simple hempel column. any glassblower can make one for cheap.

> isomerisation, peracid oxidation,and reduction with al/hg.

attention, that will give the n-methyl derivate! better do the oxime
thing and then reduction with al/hg.

[cavos]

Right, thanks.
Today I have become my delivery of NaI and NaBr.
I got some dmso analitical grade (100 Ml).
I don´t know what to do with this shit and I thinked I could try iodination throug HI in situ.How many NaI should I use for 100 Ml DMSO and 5 or 10 ml Dillseed oil?

[Vitus_Verdegast]

Use phosphoric acid instead sulfuric acid to make HI, sulfuric acid will oxidize HI to I₂.

Also, your dillseed oil will contain at most 40% dillapiole if it's the Indian variety (anethum sowa) so you really need to distill it. I doubt that using the essential oil will work.

[starlight]

This is not easy to get to work in my experience. I attempted it a couple of times, but gave up in favour of making the nitrostyrene and then reducing.

Without some proper lab equpt. like scales, distillation apparatus, you will probably end up wasting countless hours and never knowing where you went wrong.

Good luck!