1.) "Once you've got it at 104C start the stop watch and do it for 4 hours. At 104C, a small amount of distillate will come over".
Does the distillate come over during the 4 hours or just once it reaches 104C? AT 104°C, not before, not on the way towards, AT.
3.) "Filter off these Ammonium Chloride Crystals".
Are these needed, or just recycled for later use?
Save them if you want to. They won't be needed until the next time.
4.) "It may be a little wet, but if you let it crystallize hot (spontaneously in the flask with heat) it should be fairly dry".
At what temp?
This means it will crystallize hot. It should do it on its own "let IT crystallize hot".
Step:3
1.) "Drip the Safrole/DMF Mix into the solution at room temp (30C) over 30 min. time".
Should the contents in the flask be at 30C, or should the Saf/DMF mix be at 30C? If the Saf/DMF, what temp should the DMF/p-Benzo/pdc12 mix be at?
Just drip it in at room temperature.
2.) "The reaction mix was flooded with slightly acidic water".
Is this done by pouring out the contents in the flask into a container containing the acidic water? If so what type of container?
Flooding generally means adding to the flask. You can do it the other way if you prefer. Glass container with sufficient capacity will be fine.
3.) "This is when it's nice to have a Big Sep Funnel".
What size(capacity) funnel is good to have?
Any size will work. If it won't all fit in the sep funnel, pour off the acid water layer as best you can, then use the sep funnel for the last amount. Do the same thing for extracting with DCM.
4.) I read in Introduction to Organic Laboratory Techniques that an extraction solvent is poured into the Sep funnel along with the solution. Is it necessary to use an extraction solvent for this process? If so, what is the solvent needed?
DCM. That's what is meant by extracting with DCM.
5.) "Keep the DCM washes - They contain the goods".
What are the "goods" referring to?
The goods are the good stuff. Not the bad stuff. Add the DCM to the organic layer you seperated before extraction.
6.) "Now wash the DCM/Organic layer with 2x150ml 10% NaOH".
Should this wash be done the same exact way as the preveous wash with the DCM?
The previous step was NOT a wash, it was an extraction. Washing removes crap/garbage. Extraction is removing the "goods" from the garbage.
7.) "you can stop here and wait for another day - put the DCM/Organic Layer into the freezer".
Is the DCM/Organic Layer MDP2P?
It is a combination of MDP-2-P and other organics/DCM.
Step:4
1.) "If your safrole comes over at 130C then your ketone will come over at 155C".
How long after the DCM comes over should I expect to collect the ketone?
However long it takes you to turn the heat up. It is a tradeoff: the faster you turn the heat up, the quicker it will distill, but the less pure it could be. No need to be really slow, but don't just crank it up to max or it will bump all over.
2.) "Release the vacuum at the pump/aspirator and change the flask quickly - you may just dump it out, rinse it once with acetone, or IPA - and put it back".
Is the DCM what's being dumped out?
It could be safrole, water, or whatever. Just dump it out unless it is alot of safrole. Should only be a few drops if any.
3.) Can the safrole that comes over be reused?
Again, it should be just a few drops. Save it if you want, but easier to just discard.
Step:5
1.) "Basically here the AL203 is being destroyed, the water is reacting with the AL203 to form AL(OH)3 and H2".
What causes the destroying of the AL203? The water, the Hgsalt, the spatula, or athe combination of all?
It is Al2O3, not Al203 (the letter O, for Oxygen). What it means is the oxidated Aluminum (like rust) is being destroyed, exposing the Aluminum so it can react with your reagents. The mercury is destroying the oxidation (Al2O3). Since it is happening under solvent, it won't re-oxidize unless exposed to air.
2.) On a past post(can't seem to find link now) BrightStar said, "Use a small spatula instead of Hg salt". Does this mean that Hg salt is not needed at all. If not, how small of a spatula is needed? In order to stir flask contents, wouldn't this spatula have to be super small?
A spatula is like a flat scoop. A tool, not a replacement for Hg. Like a half cup of sugar, this means a small spatula of HgCl2. Not a precise measurement, but good enough for this purpose.
3.) "When amalgamation is complete, pour out the water into the milk jug".
Do the AL pieces remain in the flask, or are they poured out into the jug as well?
Pour out the water. That's what it says. Doesn't say pour out the Aluminum, so keep it in flask. Do this quickly, it isn't crucial since you will be doing an acid base later anyway. It could also be left as it is, just skip that part.
4.) "Pour in another ~350ml of water and carefully shake the flask to stir up the contents. Pour it out into the jug Do it again with another ~350ml of water".
Before it's poured into the jug, should it sit for 15-30 mins. also? If the Hg salt is, in fact needed, is more added to the 350ml of water?
Just skip the washes if it is causing you problems. Or do it as BrightStar writes. The Hg is needed to remove the Al2O3, once it is removed, the Hg isn't needed unless the Al reoxidizes. That is why you have to work fast here. Or just skip it and leave the Hg in.
5.) "Dump out as much of the water as you can in 10 seconds or so - then immediately go to the next step".
Is this the water dumped out out from the 2nd wash?
Wow, I thought it was pretty straight forward here. The washes are just to remove the Hg. Mercury is a deadly poison. It is a safety issue. Remove it now, or remove it later, either way.
6.) "Now drip this in 25ml of 25% NaOH solution over several minutes".
Should the MethylAmine/Ketone mixtuer drip into the NaOH solution, or should the NaOH drip into the MethylAmine mixture? And should the flask already be sitting in the cool water bath?
The lye is added to the Aluminum solution. Just have that ice bath ready.
7.) "Add the 2nd clear yellow liquid to the first. Do this several times, or until the clear liquid is no longer yellow ".
How much of this yellow liquid is good to have? How much should it yield?
It doesn't matter, just do it until the liquid is clear. This means you got all that was there to get.
8.) "Set up for vacuum distillation (Boiling Stones) but we're not going to distill. We are going to evaporate the Isopropyl Alcohol from the reaction contents".
Is this "reaction contents" referring to the yellow liquid?
The reaction contents are what you made. You are removing the IPA from it. The IPA was the alcohol that held your freebase MDMA.
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