Author Topic: Methylamine.HCl red. amin. questions  (Read 4653 times)

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nitrous351

  • Guest
thanks for clarification
« Reply #20 on: October 28, 2003, 11:38:00 AM »
SWIN has been using w/w calculations, but he wanted to make sure he was doing it correctly. He kinda assumed it wasn't v/v since it's difficult to measure the volume of a solid when compared to a liquid (i.e. try to make a 10% NaOH solution using v/v measurements). I think that one weakness of the Hive is the need to use molarities when making stock solutions instead of w/w.... or at least state in your writeup that your solutions are w/w. peace


hypo

  • Guest
nope
« Reply #21 on: October 28, 2003, 11:45:00 AM »
it's your weakness. % is always w/w, we even learned that in highschool.
(well, maybe in backwards america things are different...)


killerbeezzz

  • Guest
Water and MDMA?
« Reply #22 on: October 09, 2004, 12:04:00 AM »
So when you tittrate the salts it ends up in the water layer and then you just evap the water to get the crystals?  Could a rotovap be used to help evap the water?

DoctorFeelgood

  • Guest
Forget evaporating.
« Reply #23 on: October 09, 2004, 09:53:00 AM »
I agree with OC. evaporate the HCL water ??? This is nonsens. Pour HCL/np into clean sepfunnel and sep off the bottom HCL layer, which contains the base in its saltform. Then pour the HCL back into you cleaned sepfunnel and slowly add enough e.g. 20% NaOH to bring the PH up (>12). The solution will turn milkywhite and you will see the base falling out, it settles to the bottom of your sepfunnel.
Sep off base, extract remaining waterlayer once with DCM to get everything out. Combine DCM with base and strip off DCM on waterbath.
Now you have 2 options:
1)You can distill the base under reduced pressure (bp 150-155 C in my case), to get a waterwhite and clean base (higherboiling impurities removed, dark redish trash remains in flask). Then you can dissolve the clean base in e.g. xylene and gas it. This is how i do it. If you want maximum yield you can skip the distillation.
2) Dissolve it like it is in e.g. xylene and gas.

killerbeezzz

  • Guest
If the salt is there
« Reply #24 on: October 16, 2004, 08:57:00 AM »
If the salt is there why go threw all the extra steps?  SWIM would think that it would be easier just to evorate the water and get the MDMA out.  Does it give you a cleaner product to redisolve it in the NP then gass?

DoctorFeelgood

  • Guest
this is no 'extra' work
« Reply #25 on: October 19, 2004, 01:18:00 AM »
this is no extra work, this is the normal labcycle. if you skip these steps you will get a 'product' which i sure do not want to eat. you should go for purity, because these chemicals are not edible and therefore you must do these steps. some like to exclude the distilling of the freebase, but an A/B is a must. 8)

ranxerox

  • Guest
Color change
« Reply #26 on: October 20, 2004, 04:33:00 AM »
If you try to reduce the volume of water by evaporation, the heat will cause the flask contents to turn a beautiful violet color, then darken to a very deep purple, almost black. Then after crystalization the formed crystals will have the same purple color. The color can be removed by recrystalization.

Recrystalization is almost always necessary with titrated products. Gassing is a bad nightmare compared to titration.

psychokitty

  • Guest
Cinnamaldehyde?
« Reply #27 on: October 20, 2004, 05:30:00 AM »
Has anyone considered using cinnamaldehyde in the Al-Hg reductive amination to see if it works equally well at creating the same reaction conditions that using MD ketone does?

My thought is that cinnamaldehyde could be appied to a practice run. This could eliminate the risk of wasting valuable chems during a standard newbee Al-Hg reductive-amination familiarization process.