How to make methylamine gas?
Synteza MDMA za pomocą NaBH4 z MDP2P
- Thread starter G.Patton
- Start date
Your 300g methylamine gas is it mean use cas 593-51-1 dissolve in methanol?
- By G.Patton
Hello, no. Every substance have own weight. Methylamine has gas form at normal conditions. 300g of methylamine free base (gas) has to be dissolved in methanol.
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- By Win Win
A vacuum distillation setup is prepared. Methanol, DCM, water and other low boiling substances are distilled off at 130 °C firstly. Then, a heater is set at 165 °C, little drops of MDMA oil are condensated and seen around 140-145 °C; at 160-165 °C (20-18 mbar) MDMA oil is distilled intensively. The clean MDMA free base distillation yield is ~ 1.0 L.
A membrane vacuum aspirator is sufficient to distill off water, methanol and other low boiling substances from the reaction mixture. A decent vacuum pump is recommended to distill MDMA free base.
This step can i use rotaryevaporator?
A membrane vacuum aspirator is sufficient to distill off water, methanol and other low boiling substances from the reaction mixture. A decent vacuum pump is recommended to distill MDMA free base.
This step can i use rotaryevaporator?
- By William D.
A very high initial temperature for these solvents, especially using a vacuum. And it is better to exclude water with drying agents if you want to get the maximum yield. In addition, you can extract amine in the water layer and already work with the water layer, the dcm will take the impurities, and you can avoid distillation if your raw materials have been of good quality.
Methylamine gas (MeNH2) 300 g is dissolved in chilled 3000 g methanol (MeOH; -17-20 °C) in 20 L reactor, equipped with thermometer and overhead stirrer. The mixture is cooled down to 5 °C. The stirrer is turned on and MDP2P 1000 g is added.
In my country methylamine 44%in methanol liquid ready made available
So just add liquid to flask and mantain 5 c temp add mdp2p
I'm i right ?
Because I don't have deep fridge so I can't methanol (MeOH; -17-20 °C
Plz help
@G.Patton
In my country methylamine 44%in methanol liquid ready made available
So just add liquid to flask and mantain 5 c temp add mdp2p
I'm i right ?
Because I don't have deep fridge so I can't methanol (MeOH; -17-20 °C
Plz help
@G.Patton
Methylamine in methanol 30% readymade
Sodium borohydride (NaBH4) 100 g is added in portions, one teaspoon per ~5 min, H2 gas bubbling has to disappear before next addition (wash down with methanol). Temperature is maintain between 8-10 °C. Sodium borohydride (NaBH4) addition is taken 2-7 h. The mixture is stirred for 2 days. The stirring time can be reduced to 4 h for people in a hurry, 10-20% will be lost.
@G.Patton
AVAILABLE
in my country so i need to add mdp2p in Methylamine in methanol 30% then do thisSodium borohydride (NaBH4) 100 g is added in portions, one teaspoon per ~5 min, H2 gas bubbling has to disappear before next addition (wash down with methanol). Temperature is maintain between 8-10 °C. Sodium borohydride (NaBH4) addition is taken 2-7 h. The mixture is stirred for 2 days. The stirring time can be reduced to 4 h for people in a hurry, 10-20% will be lost.
@G.Patton
DCM 200 mL is added to the reaction vessel with water layer and the mixture is stirred for 10 min. The stirrer is stopped and reaction mixture is left 30 min. DCM with the rest MDMA freebase will settle on the vessel bottom. Organic layer is drained out and extracts are combined. There is ~1750 mL of MDMA free base and DCM.
my qustion DCM 200 mL is added to the reaction vessel with water layer and the mixture is stirred for 10 min what is water layer in this ?
@G.Patton
my qustion DCM 200 mL is added to the reaction vessel with water layer and the mixture is stirred for 10 min what is water layer in this ?
@G.Patton
In this writeup
PS I must mention here that those 108 grams were the most potent ever felt by the elves, by the way.......
360 ml mdp2p to make
108 gm mdma it's not 90 % yeild you said it's 90 % I read everything in this link it show 108 gm mdma with mdp2p
@G.Patton help
Gyrogearloose:
Well guys From 360 ml of MDP2P to begin with the elves got 108 grams of the crystals, using the method for them of adding HCL to the freebase oil then adding the cold acetone, boom fun to watch the crystals comeinto chunks then .The elves love it....PS I must mention here that those 108 grams were the most potent ever felt by the elves, by the way.......
360 ml mdp2p to make
108 gm mdma it's not 90 % yeild you said it's 90 % I read everything in this link it show 108 gm mdma with mdp2p
@G.Patton help
- By G.Patton
Because elves had to add acetone at first and then HCl to avoid overheating and local overacidification which decrease yield. Also, elves could evaporate mother liquor from crystals filtration for 1/2 and get more product there.
108g of MDMA HCl from 360 ml of MDP2P is just 28% yield. Pretty low.
108g of MDMA HCl from 360 ml of MDP2P is just 28% yield. Pretty low.
- By imcoc2
man your post on this is same and elves do same things you do why you said 90+ YEILDS
HELP ME WITH THIS MAN HE DO SAME THINGS YOU DO IN THIS SYNTHIS
I SEE NO DIFFRANCE MAN
These quantities are in weight! (So: gram or kg).
Following starting quantity is 25 kg P:
Prepare 6x20 L yerrycans in wich you can fill each 12,5 L cooled (-20 C) MeOH. In each yerrycan you dissolve 1,25 kg methylamine in the cooled MeOH.
Let the MethylAmine dissolve in the -20 C cooled MeOH wich you already put in the freezer one night before! Use a upside down laying gastank with MA (30-45' angle)and fill with a thick synthetic black rubber hose the liquid-MA as deep as possible in the MeOH. SLOWLY! It takes ca. 10 min., per yerrycan.
The yerrycan stands on a digital balance, so you know the weight added. Surround the hose with a wet towel at the filling opening of the yerrycan for the unhealthy smell.
When ready fill all the yerrycans in the reactiontank.
[Add in case of (MDA) now the AAcetate( in methanol) instead of the MeNH2 !].
Cool now the reactiontank to +5 C and start the mixer anticlockwise, so the fluid circulates from bottom to top. This way no air is mixed in, so less oxidation. Add at +5 C the 25 L. MDP2P .(pre-cooled).
Start then directly (because a slow reaction starts already), every ca. 5 min, adding the NaBH4, ca. 3 soupspoons per time. Use a funnel and wash every time with a little methanol. Keep all holes closed inbetween or it stinks!
Because of the excessive cooling the temp. will not rise much, only to +15 C. Wait again till ca. +7 C to add again. Are you impatient and add to quick, then the mix will start heating,evenso boiling! This may never occur,then your product will be lost !
This process takes ca. 7 hours. Ending temp. will be ca. 25 C. Stop after 7 hrs. the cooling and let react with mixer on for 36 hours.
After this time, you prepare 200 L clean water, which you mix with 2 liter 33% HCl solution.
This mix you add to the cooling tank (fast), then you messure the pH, should be between 11,5 and 12. (If you add coincidently too much acid,you will see greenish fat form in and on the fluid. Stop after 10 min. the mixer and let the raw brown base precipitate 30 min to the bottom and tap off the base through the valve at the bottom. Stop tapping when you see lighter color (water) coming.
Add now 3 liter methylenechloride (dichloromethane=CH2Cl2) to the tank, mix 10 min., stop the mixer, wait again 30 min. and tap off the rest of the base, now diluted in the CH2Cl2.This gives totally ca. 43 L raw base.
Now we remove the CH2Cl2, Methanol and the water in a simple distillation setup, without vacuum, with magnetic mixer/heater, mixerpin teflon, glassware with NS29 connections ( 20 L 2-neck flatbottom flask PYREX!, thermometer, cooler 60 cm, glas-alonge and 10 L collecting flat-bottom erlenmeyer flask).
Start at 35->55 C for CH2Cl2, then 55->85 C for methanol and 130 C for all the water. Re-use the CH2Cl2 and the methanol! Now you are left with ca 28 L half-clean base.(light brown).
Now we will clean the raw base by 2 times recrystallisation with acetone 98%, (m)ethanol 98%, and after that washing min. 3 times with acetone 98%. Use 20 L P.P. plastic buckets to do this.
Mix 5 L base (cold) and 10 L icecold acetone. Leaf inductionmotor-mixer on. Bubble HCl-gas 99% through with 1 meter StainlessSteel pipe, (inner diameter min 5mm) until white crystals form. Stop when pH= 7,3 and start with the next 5 L base. The first one will rise again to ca. pH=8,0. Later you can bubble again a littlebit HCl-gas through until again pH=7.0 . Let the crystals precipitate and pour the upper acetone off.
Re-dissolve the wet crystals now in the minimum quantity of HOT(nearly boiling) (m)ethanol in a metal bucket (because its hot !) until you see no more crystals, so you have a saturated solution in (m)ethanol!
Pour 5 L of this solution back in the plastic bucket, and add 5 L -15 C Acetone. When cooling down, you will see crystals form again,in a dirty solution. Wait until no more crystals come, pour off again and dissolve again in hot (m)ethanol. Do this as many times until you have snowwhite crystals. Dry on glasplates on the floor with blower.
You now have H(M)ONEY in the Bank.
PS I must mention here that those 108 grams were the most potent ever felt by the elves, by the way.......
Before ,you mentioned me they get 342 gram out of 400 gram MDP2P. What was that? MDA I thought. When Billy does this, he always get min. 90 gram to max. 122 gram out of 100 gram MDP2P (MDMA !).with 99% HCl-gas!Like you make toothpaste instead of crystals...At the end its heavy to mix around!
So again, distill your SUSPECTED TO BE MDP2P always one time, to get min 95% and check eventually with any possible means if you really have MDP2P.
I got the impression that many people here do'nt work with real min 95 % MDP2P, but contaminated product. Billy works with for sure 98% MDP2P ! Checked,Checked and Checked!
I wait with the Pressure stuff until I have the feeling that the one's who work on this, do'nt need anymore help, otherwise everybody runs to the pressure Pots.
Hey, how about the P2P to Meth stuff? ANYBODY any NEWS? Get famous,post it!
Billy looks now at a solution of P2P,5A Molsieves,MeOH+10%MeNH2, which stood for a week.It turned slowly to a dark GREEN fluid. With a bit white precipitate between the molsieves (Alu-salt?) Can the Alu ions in the molsieves do that in a week?
Should he filter and add then the NaBH4 or should the Alu already have reduced (part of) it? INPUT please. MUCH MORE INPUT!
Sorry for making you look bad sir, it was the elves fault as you can see. Pointed ears somehow miss things round ones hear... Same goes for heads...as for the crystalization method they just neutralized the oil with 38% HCL and then added cold acetone and the boulders rolled on into being, minimum cleaning needed.
HELP ME WITH THIS MAN HE DO SAME THINGS YOU DO IN THIS SYNTHIS
I SEE NO DIFFRANCE MAN
These quantities are in weight! (So: gram or kg).
Following starting quantity is 25 kg P:
Prepare 6x20 L yerrycans in wich you can fill each 12,5 L cooled (-20 C) MeOH. In each yerrycan you dissolve 1,25 kg methylamine in the cooled MeOH.
Let the MethylAmine dissolve in the -20 C cooled MeOH wich you already put in the freezer one night before! Use a upside down laying gastank with MA (30-45' angle)and fill with a thick synthetic black rubber hose the liquid-MA as deep as possible in the MeOH. SLOWLY! It takes ca. 10 min., per yerrycan.
The yerrycan stands on a digital balance, so you know the weight added. Surround the hose with a wet towel at the filling opening of the yerrycan for the unhealthy smell.
When ready fill all the yerrycans in the reactiontank.
[Add in case of (MDA) now the AAcetate( in methanol) instead of the MeNH2 !].
Cool now the reactiontank to +5 C and start the mixer anticlockwise, so the fluid circulates from bottom to top. This way no air is mixed in, so less oxidation. Add at +5 C the 25 L. MDP2P .(pre-cooled).
Start then directly (because a slow reaction starts already), every ca. 5 min, adding the NaBH4, ca. 3 soupspoons per time. Use a funnel and wash every time with a little methanol. Keep all holes closed inbetween or it stinks!
Because of the excessive cooling the temp. will not rise much, only to +15 C. Wait again till ca. +7 C to add again. Are you impatient and add to quick, then the mix will start heating,evenso boiling! This may never occur,then your product will be lost !
This process takes ca. 7 hours. Ending temp. will be ca. 25 C. Stop after 7 hrs. the cooling and let react with mixer on for 36 hours.
After this time, you prepare 200 L clean water, which you mix with 2 liter 33% HCl solution.
This mix you add to the cooling tank (fast), then you messure the pH, should be between 11,5 and 12. (If you add coincidently too much acid,you will see greenish fat form in and on the fluid. Stop after 10 min. the mixer and let the raw brown base precipitate 30 min to the bottom and tap off the base through the valve at the bottom. Stop tapping when you see lighter color (water) coming.
Add now 3 liter methylenechloride (dichloromethane=CH2Cl2) to the tank, mix 10 min., stop the mixer, wait again 30 min. and tap off the rest of the base, now diluted in the CH2Cl2.This gives totally ca. 43 L raw base.
Now we remove the CH2Cl2, Methanol and the water in a simple distillation setup, without vacuum, with magnetic mixer/heater, mixerpin teflon, glassware with NS29 connections ( 20 L 2-neck flatbottom flask PYREX!, thermometer, cooler 60 cm, glas-alonge and 10 L collecting flat-bottom erlenmeyer flask).
Start at 35->55 C for CH2Cl2, then 55->85 C for methanol and 130 C for all the water. Re-use the CH2Cl2 and the methanol! Now you are left with ca 28 L half-clean base.(light brown).
Now we will clean the raw base by 2 times recrystallisation with acetone 98%, (m)ethanol 98%, and after that washing min. 3 times with acetone 98%. Use 20 L P.P. plastic buckets to do this.
Mix 5 L base (cold) and 10 L icecold acetone. Leaf inductionmotor-mixer on. Bubble HCl-gas 99% through with 1 meter StainlessSteel pipe, (inner diameter min 5mm) until white crystals form. Stop when pH= 7,3 and start with the next 5 L base. The first one will rise again to ca. pH=8,0. Later you can bubble again a littlebit HCl-gas through until again pH=7.0 . Let the crystals precipitate and pour the upper acetone off.
Re-dissolve the wet crystals now in the minimum quantity of HOT(nearly boiling) (m)ethanol in a metal bucket (because its hot !) until you see no more crystals, so you have a saturated solution in (m)ethanol!
Pour 5 L of this solution back in the plastic bucket, and add 5 L -15 C Acetone. When cooling down, you will see crystals form again,in a dirty solution. Wait until no more crystals come, pour off again and dissolve again in hot (m)ethanol. Do this as many times until you have snowwhite crystals. Dry on glasplates on the floor with blower.
You now have H(M)ONEY in the Bank.
Gyrogearloose:
Well guys From 360 ml of MDP2P to begin with the elves got 108 grams of the crystals, using the method for them of adding HCL to the freebase oil then adding the cold acetone, boom fun to watch the crystals comeinto chunks then .The elves love it....PS I must mention here that those 108 grams were the most potent ever felt by the elves, by the way.......
LaBTop:
Gyro, I'm a bit worried here. This is about MDA? Did your Elfes use 33% HCl or bubbled 99% HCl gas?Did they NOT pass the pH 7 border? If they used 33%, there will be another substantial part of their product dissolved in the 66% water part! Do'nt throw it away... Boil it dry, and look, next present...Before ,you mentioned me they get 342 gram out of 400 gram MDP2P. What was that? MDA I thought. When Billy does this, he always get min. 90 gram to max. 122 gram out of 100 gram MDP2P (MDMA !).with 99% HCl-gas!Like you make toothpaste instead of crystals...At the end its heavy to mix around!
So again, distill your SUSPECTED TO BE MDP2P always one time, to get min 95% and check eventually with any possible means if you really have MDP2P.
I got the impression that many people here do'nt work with real min 95 % MDP2P, but contaminated product. Billy works with for sure 98% MDP2P ! Checked,Checked and Checked!
I wait with the Pressure stuff until I have the feeling that the one's who work on this, do'nt need anymore help, otherwise everybody runs to the pressure Pots.
Hey, how about the P2P to Meth stuff? ANYBODY any NEWS? Get famous,post it!
Billy looks now at a solution of P2P,5A Molsieves,MeOH+10%MeNH2, which stood for a week.It turned slowly to a dark GREEN fluid. With a bit white precipitate between the molsieves (Alu-salt?) Can the Alu ions in the molsieves do that in a week?
Should he filter and add then the NaBH4 or should the Alu already have reduced (part of) it? INPUT please. MUCH MORE INPUT!
Gyrogearloose:
e gads, sir you were right on, it was hiding in the water........I was thinking it was small but powerful in a new way. This is high octaaane stuff. Its by far the best yet for the elves. Additional 232 grams were recovered thanks to your highness sir laBtop.Sorry for making you look bad sir, it was the elves fault as you can see. Pointed ears somehow miss things round ones hear... Same goes for heads...as for the crystalization method they just neutralized the oil with 38% HCL and then added cold acetone and the boulders rolled on into being, minimum cleaning needed.