01-22-02 14:55
No 259557
These are a few questions I have on BrightStars synth.
Due to limited time, I have listed about half the questions I have written, but will be back later to post the rest.
Thanks in advance for any info.
Step:2
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? Is the methylal and methylformate needed at any point?
2.) "Within 30 minutes or so - liquid should start coming over".
What is the contents of this liquid?
3.) "Filter off these Ammonium Chloride Crystals".
Are these needed, or just recycled for later use?
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?
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?
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?
3.) "This is when it's nice to have a Big Sep Funnel".
What size(capacity) funnel is good to have?
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?
5.) "Keep the DCM washes - They contain the goods".
What are the "goods" referring to?
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?
7.) "you can stop here and wait for another day - put the DCM/Organic Layer into the freezer".
Is the DCM/Organic Layer MDP2P?
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?
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?
3.) Can the safrole that comes over be reused?
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?
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?
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?
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?
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?
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?
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?
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?
(Hive Bee)
01-22-02 17:35
No 259636
Since swim is in a good mood here is some help for ya. But in the future you should UTFSE all these question were asked before.You gotta read to learn.
step 2----- skip it altogether Use methylman's nitromethane al/hg synth a whole lot easier. It's on rhodium's site. Search for it you'll find it.
Step 3----- Room temperature is room temperature. Average room temp is 30. whatever your is will be fine.Pour it in a separatory funnel 2000ml.Just follow the synth.The "goods" is your product. Wash like it says to wash.
step 4----- Your ketone will come over when the temp is right for it to come over. there is no real time to go by.You'll have to find the rest of step 4 on you own.
step5------the water and the hg salt the spatula is for mixing it!!!hello. Bs said you can use a small spatula of hg salt. YOU NEED THE HG SALT.
I think swim helped you enough do a little searching you'll find the answers.
(Old P2P Cook)
01-22-02 19:06
No 259678
Yes, questions like this should be in the Newbee Forum.
Re. Step 2: see Post 209576 (terbium: "Re: Methylamine; So many problems? Is it the Altitude", Newbee Forum)
(Hive Addict)
01-22-02 19:28
No 259692
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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(Stranger)
01-23-02 09:36
No 259910
I realize this probably should have been in the Newbee Forum, but I read plenty of past post in A.D. simular to this and thought it was in the appropriate forum. Future post of such content will be in their appropriate spot, but for now please allow me to finish with my last few questions. And thanks, noj. Made things much more clear.
Step.5)(cont.)
9.) "After the alcohol is gone, take the brown oil that is left and put it into 500ml of ~0.5m HCI solution".
Should this be done in the flask or a seperate jug?
10.) "Wash the aqueous layer again with 30ml of DCM, and repeat the process".
How many times?
11.) "Now, slowly add 50ml of 25% NaOH solution to the aqueous layer?
Again, is this done in the flask?
12.) "A light brown oil will fall out of the solution".
Is "fall out" the same thing as settling to the bottom?
13.) "Pour off the top Aqueous layer, and KEEP THE DCM THIS TIME".
The DCM in the poured off aqueous layer?
Step:6
1.) "Get a fresh bottle of 91% Isopropyl Alcohol, and pour out approximately 100ml".
Into the distillation flask?
2.) "Pour off the IPA, and put more fresh MgSO4 into it (about 100ml worth)".
Is the IPA the top layer? And does "it" refer to the settled out MgSO4?
3.) "After three times you will have 'Dry" IPA".
Is the 'Dry' IPA a collection of aqueous layers from the IPA/MgSO4 mixtures that were just shaken?
4.) "Pour it into the flask that contains the MDMA oil, and drop the stirbar into it".
Is the MDMA oil what was referred to earlier as the New Castle looking oil?
5.) "Under vacuum, the solution should never get above 70C".
Isn't it already set up for vacuum distillation? If so then why warn not to got above 120C if, in fact, it shouldn't go above 70C?
Replies are much appreciated!
(Hive Addict)
01-23-02 12:14
No 259975
9.) "After the alcohol is gone, take the brown oil that is left and put it into 500ml of ~0.5m HCI solution".
Should this be done in the flask or a seperate jug?
Since you will be washing it next, use a seperate container, or a sep funnel.
10.) "Wash the aqueous layer again with 30ml of DCM, and repeat the process".
How many times?
2 is enough.
11.) "Now, slowly add 50ml of 25% NaOH solution to the aqueous layer?
Again, is this done in the flask?
See above.
12.) "A light brown oil will fall out of the solution".
Is "fall out" the same thing as settling to the bottom?
Basically. When it is acidic, it will stay in the water as a solution. Once you basify it, it can no longer stay in the solution, so it seperates, and falls to the bottom (it is more dense than water).
13.) "Pour off the top Aqueous layer, and KEEP THE DCM THIS TIME".
The DCM in the poured off aqueous layer?
DCM is also more dense than water, and will be on the bottom. Your MDMA freebase is also contained within the DCM. If you are using a sep funnel, you can drain the bottom layer easily. Otherwise, you will have to decant (pour off) the water layer (on top) off. Carefully. Sep funnels are deigned for this purpose, it makes it easy to seperate different layers of fluids.
1.) "Get a fresh bottle of 91% Isopropyl Alcohol, and pour out approximately 100ml".
Into the distillation flask?
2.) "Pour off the IPA, and put more fresh MgSO4 into it (about 100ml worth)".
Is the IPA the top layer? And does "it" refer to the settled out MgSO4?
3.) "After three times you will have 'Dry" IPA".
Is the 'Dry' IPA a collection of aqueous layers from the IPA/MgSO4 mixtures that were just shaken?
This is a process to remove the water from the IPA. It can be done seperately from everything. Use whatever is handy, even a drinking glass is ok. Things are easier to understand if you just follow it as you go. But I understand you want to be certain of everything. The IPA will stay fluid, and the MgSO4 will absorb the water like a sponge. The MgSO4 gets filtered out. Pour the solution through a coffee filter and funnel into a new glass (anything), and repeat with fresh (dry) MgSO4.
4.) "Pour it into the flask that contains the MDMA oil, and drop the stirbar into it".
Is the MDMA oil what was referred to earlier as the New Castle looking oil?
Yes. It was what you got from question 13 above.
5.) "Under vacuum, the solution should never get above 70C".
Isn't it already set up for vacuum distillation? If so then why warn not to got above 120C if, in fact, it shouldn't go above 70C?
120°C if you are not using vacuum, 70°C if you are.
crucify the ego before it's far too late
and you will come to find that we are all one mind