Methamphetamine synthesis from P2P by NaBH4 reduction. Medium-Scale.

[btcboss2022]

Introduction.​

I represent to BB audience Methamphetamine synthesis method of 1-phenyl-2-propanon (P2P) reduction by NaBH4. Following method allows obtaining and large batches of product. The hardest problem of this method is the heat generating during exothermic reaction of imine reduction. Extremely important keep temperature in described frames and keep all reagent and reaction atmosphere dry (use drying tubes with CaCl2). Also, manipulations with NaBH4 is quite dangerous and take a lot of attention because this reagent has toxic effects, reacts with water and alcohols with releasing enormous amount of hydrogen and form the corresponding borate, it may cause an explosion, burns and injuries. You have to use chemical glass, gloves, chemical coat and respirator.​

Equipment and glassware:​

• Ceramic mortar;​
• 2 L (x2), 0.5 L (x2) and 200 ml (x2) beakers;​
• 2 L (x2) and 10 L Erlenmeyer flask;​
• Measuring cylinder for 100 ml;​
• 2 L three-necked round bottom flask with plugs;​
• 2 L round bottom flask with vacuum quickfit or Schlenk flask;​
• 0.5 L Simple dropping funnel with Claisen flask and drying tube or 0.5 L equal pressure dropping funnel;​
• 1 L Separator funnel;​
• 2 L Evaporation flask;​
• Pyrex dish 0.5 L;​
• Magnetic stirrer with heating plate;​
• Retort stand and clamp for securing apparatus;​
• Silicone-oil bath;​
• Icecubes/methanol bath (-10 °C) or Mashed ice with salt (-10 °C);​
• Laboratory scale (1 g-1 kg is suitable);​
• Oven;​
• Laboratory grade thermometer (-20 °C to 200 °C) with three-necked flask adapter;​
• Aspirator;​
• HCl laboratory generator;​
• Drying tube x2;​
• Rotavap machine with water bath;​
• Filter paper.​

Reagents:​

• 138 gram P2P (1 mole) (1-phenyl-2-propanone);​
• 10% Methylamine in Methanol (w/w) - 1000 ml with 100 g MeNH2 (~3 moles);​
• Magnesium Sulfate - 36 g (MgSO4·7H2O, oven dry at 300 °C for 2h MgSO4·1H2O) [For drying MeOH/MeNH2 solution];​
• Silica Gel (3-5 mm balls) - 200 ml (dry at 300 °C/2h, they will darken!) [For absorbing 2 mol H2O during rxn];​
• 15 gram NaBH4 as a reducing agent for the formed (water-free!) imine;​
• 5-7 L distilled water + ~5 L distilled water to filling rotavap machine bath;​
• 1 L Dichloromethane (DCM);​
• 0.5 L Acetone.​

Important: the reaction is very sensitive to any water (fluid or vapour in the air!).

Note: hold all manipulations in pull out probe or under exhaust hood; methylamine is a rather toxic substance, do not let its vapors enter the respiratory tract. Using respiratory mask is required. Inhalation of methylamine causes severe skin irritation, eyes and upper respiratory tract. Firstly, leads to excitement and then to depression of the central nervous system. Death can occur from respiratory arrest.​

Procedure.​

Precursors drying.
First quickly crunch your pre-dried (oven, 300 °C, 3 hrs.) dry MgSO4 to pop corn shaped rocks in a mortar, sieve the powder out, and directly put the rocks under max. mixing in the Methanol/Methylamine mix (1000 ml) and close the pot to let no water from the air in. Keep mixing for 10 minutes, then all the water will be taken up to the MgSO4. Let stand and wait till all the MgSO4 is on the bottom. Now quickly tap off the now dry MeOH/methylamine (MA) mix in a 2 L three-necked round bottom flask and close that one. Wash directly your empty pot with lots of water, to remove the smell of methylamine, so you can safely store it.
​

Synthesis.

Now add the 200 ml (measure in beaker, neglect the free spaces) dry Silicagel beads (2-5 mm) and a magnetic mixer bar also in the 2 L flask and close again. Keep 2 L flask in Silicone-oil bath at 20 °C. Silicone-oil only slowly warms up! Do not apply heat now, it's only meant as a cooling medium in this stage. Now add slowly via a dropping funnel the 138 g P2P to the 2 L flask under strong mixing. The temperature rises to 23 °C during the (water-free) Imine forming. The water from this reaction is taken up by the dried Silicagel! This takes 30 minutes. Let, then mix for another hour. The reaction mix color changes from light yellow to coffee+milk color. Temp 23 °C.​

View attachment 2944 ​

Stop mixing after this 1 hour and pour the fluid off into a 2 L glass erlenmeyer with flat bottom and add a mixbar. The remaining Silicagel is washed 3 times with 50 ml dried (use silicagel) methanol, to catch the remaining Imine, and those 2 x 50 ml is also poured into the 2 L erlenmeyer. Now put the 2 L erlenmeier on magn.mixer, in an icecubes/methanol bath (-10 °C) (or mashed ice with salt) and start strong mixing. Put a drip funnel on top of 2 L erlenmeier, in rubber ring. Now start adding, every 5 min., a teaspoonfull (flat off!) of NaBH4 in minimum methanol, wash it from funnel with minimum methanol amount. After every spoonfull, stopper the funnel loosely with a rubber stopper. This takes 2.5 hrs. Do not exceed a temp of more than 20 °C! You can add the next spoon at ±8 °C. Solution color is light clear orange/brown. Let mix in total for 8.5 h (could perhaps be lot fewer hours).​

View attachment 2945 ​

The total volume is ~1900 ml. Add then the mix to 5 L distilled water into a 10 L flask, under magn.mixing. The pH=12. Add then 500 ml DiChloroMethane (DCM) and mix strongly for 30 min. Let oil precipitate and a dark, honey-coloured layer of DCM+oil settle onto the bottom. Decant the water part with an aspirator + siliconetube. Fill the rest (water+DCM+oil) in a seperatory funnel and tap off only the DCM+oil = 550 ml. (DCM b.p. 40 °C). The leftover MgSO4 and boro salts stayed nicely in the waterpart. Then dry the DCM+oil with some dry MgSO4 and decant in 2l erlenmeier. Wash this MgSO4 with some fresh, DRY DCM and add the DCM washings to the now dry DCM+oil. Total volume DCM+oil =1000 ml, colour is honey/red.​

Producing methamphetamine hydrochloride.

Start now bubbling this 1000 ml with HCl-gas via 2 L Schlenk flask (or round bottom flask with vacuum quickfit), while this 2 L flask stands in ice bath on magn. mixer and blends vigorously. Check pH frequently, proceed until pH 6. Pour the now acidified 1000 ml in a 2 L evaporation flask and put on Rotavap machine. Spee~100 rpm, t° = 80 °C, little vacuum=0.8 bar (water-jet aspirator is enough), to hold the flask. After distillating off nearly all the DCM, suddenly the contents of the flask turns from dark honey colour to creamy milk color, and it dries out to a round cake on the bottom. Remove the ~0.5 L DCM, now in the collector flask, and hang that empty flask on again. Now put full vacuum on to remove the last traces of water.

Cleaning by 3 x recrystallization: put minimum quantity of hot (40 °C) dry DCM (or dry 98%+ ethanol) in the flask until the last remains of the dry stuff dissolves, and add 4x this DCM-quantity in the form of dry acetone. Close with stopper and put 1 hr in freezer. A solid dirty-white crystal mass is formed with a layer of dark red fluid on top of it. Decant the fluid and repeat this step another 2x and 2 hrs. You have, the last time, snow-white crystals of racemic methamphetamine hydrochloride. Dry Weight = 141.5 g, close to quantitative yield.

Methamphetamine purification.
You can use this technique or follow next advices to produce ICE meth: melt this crystal mass in an alu flat bottom pot on a heater plate at 170-175 °C. Then let this melt, very slowly, and do not go higher than necessary to melt it, or its starts smoking (you have your first quick-test then: enjoy!). Cool down to 150 °C again, really slowly, 1 °C/30 min. (regulate with your temp controller!), and you got ICE, after you let it very slowly again cool down to room temperature (with a closed lid on it!, its hygroscopic!). Advantage: you removed all the water in this process!

You can better make the sulfate salt following logical method: Let 10% H2SO4/Ethanol mix acidifying a 1:4 mix of freebase Meth/Ethanol. This is not so hygroscopic. Filter and dry the crystals.​

G.PattonHello,

After many tests using Methylamine HCL based on this method I will share the best way that I found to obtain Methamphetamine freebase in big scale:

• 966 gr P2P​
• 14 liters Methanol
• 1183 gr Methylamine HCL​
• 638gr NaOH​
• 452 gr Anhydrous Sodium Sulfate​
• 105 gr NaBH4​
• 35 L distilled water​
• 7 Liters DCM​

- Fill the reactor with the 14 L of Methanol
- With stirring dissolve the Methylamine HCL
- Put the reactor temp at 0C(not the mixture temp) and add the NaOH, the temp will increase
- Once the temp come back to 20C add the P2P, the temp will increase stir it during 45min-1 hour
- Add 252gr of anhydrous sodium sulfate
- When the mixture temp arrives to 8C start adding portionwise the NaBH4 not exceeding the 20C
- Once all the NaBH4 has been added let it mixing under 20C during aprox 2 hours until the mixture stops bubbling
- Add the water and continue mixing during 5 min
- Add the DCM and mix it during 10 min
- Stop stirring and let layers get separated
- Keep the bottom layer and discard the upper one( not profitable to extract this aqueous phase)
- Add 200gr of anhydrous sodium sulfate to the saved layer and mix it
- Filter it in Buchner Funnel
- Evaporate the DCM
- Clean and smelly Methamphetamine freebase obtained

;-)

 

[Win Win]

Hello,

After many tests using Methylamine HCL based on this method I will share the best way that I found to obtain Methamphetamine freebase in big scale:

• 966 gr P2P​
• 14 liters Methanol
• 1183 gr Methylamine HCL​
• 638gr NaOH​
• 452 gr Anhydrous Sodium Sulfate​
• 105 gr NaBH4​
• 35 L distilled water​
• 7 Liters DCM​

- Fill the reactor with the 14 L of Methanol
- With stirring dissolve the Methylamine HCL
- Put the reactor temp at 0C(not the mixture temp) and add the NaOH, the temp will increase
- Once the temp come back to 20C add the P2P, the temp will increase stir it during 45min-1 hour
- Add 252gr of anhydrous sodium sulfate
- When the mixture temp arrives to 8C start adding portionwise the NaBH4 not exceeding the 20C
- Once all the NaBH4 has been added let it mixing under 20C during aprox 2 hours until the mixture stops bubbling
- Add the water and continue mixing during 5 min
- Add the DCM and mix it during 10 min
- Stop stirring and let layers get separated
- Keep the bottom layer and discard the upper one( not profitable to extract this aqueous phase)
- Add 200gr of anhydrous sodium sulfate to the saved layer and mix it
- Filter it in Buchner Funnel
- Evaporate the DCM
- Clean and smelly Methamphetamine freebase obtained

;-)

btcboss2022Hi sir after evaporate dcm get the liquid colour like light yellow. Is it meth free base?

 

[btcboss2022]

Hi sir after evaporate dcm get the liquid colour like light yellow. Is it meth free base?

Win WinIf you followed all the steps correctly yes but there are methods more accurate to check that.

 

[Win Win]

Hello,

After many tests using Methylamine HCL based on this method I will share the best way that I found to obtain Methamphetamine freebase in big scale:

• 966 gr P2P​
• 14 liters Methanol
• 1183 gr Methylamine HCL​
• 638gr NaOH​
• 452 gr Anhydrous Sodium Sulfate​
• 105 gr NaBH4​
• 35 L distilled water​
• 7 Liters DCM​

- Fill the reactor with the 14 L of Methanol
- With stirring dissolve the Methylamine HCL
- Put the reactor temp at 0C(not the mixture temp) and add the NaOH, the temp will increase
- Once the temp come back to 20C add the P2P, the temp will increase stir it during 45min-1 hour
- Add 252gr of anhydrous sodium sulfate
- When the mixture temp arrives to 8C start adding portionwise the NaBH4 not exceeding the 20C
- Once all the NaBH4 has been added let it mixing under 20C during aprox 2 hours until the mixture stops bubbling
- Add the water and continue mixing during 5 min
- Add the DCM and mix it during 10 min
- Stop stirring and let layers get separated
- Keep the bottom layer and discard the upper one( not profitable to extract this aqueous phase)
- Add 200gr of anhydrous sodium sulfate to the saved layer and mix it
- Filter it in Buchner Funnel
- Evaporate the DCM
- Clean and smelly Methamphetamine freebase obtained

;-)

btcboss2022I use HCI gas dont have crystall come out. I change to use dropwise HCL also dont have crystall come out. What is the problem?

 

[Win Win]

With dropwise wont appears crystals at this stage, what pH you left?what do you do after this?

btcboss2022Sir i would like to ask you. When i use HCI gas is it need use ice bath?

 

[btcboss2022]

Sir i would like to ask you. When i use HCI gas is it need use ice bath?

Win WinDon't need it. Anyway I don't use HCL gas.

 

[Win Win]

Don't need it. Anyway I don't use HCL gas.

btcboss2022But i use HCL dropwise also cant get crystall out. Is it PH problem? Or my working step have problem?

 

[hunter12]

Sir this is the liquid colour after i finish all step. Is it right?

Win WinSame thing that happened to me. I think its caused by over heating the oil

 

[btcboss2022]

PH6. After i dropwise HCI Use a heating mantle to heat the liquid to 105 degrees and pour it into the tray

Win WinPH 3 and 108C

 

[Win Win]

PH 3 and 108C

btcboss2022After heating need keep it in freezer?

 

[btcboss2022]

After heating need keep it in freezer?

Win WinNo

 

[Win Win]

No

btcboss2022Alright thank you

 

[btcboss2022]

I think btcboss also uses freebase because after adding the Methylamine HCl he add NaOH to the solution, so makes essentially freebase from the HCl salt.

diogenesYes Methylamine HCL+NaOH=Methylamine freebase in my case Methylamine HCL is cheaper and I get more freebase amount with less investment.

 

[jotoy]

Yes Methylamine HCL+NaOH=Methylamine freebase in my case Methylamine HCL is cheaper and I get more freebase amount with less investment.

btcboss2022Hi
Im a little confuse. So if i buy methylamine HCL and add it in methanol with sodium hudroxide it will becaome a solution?

 

[btcboss2022]

Hi
Im a little confuse. So if i buy methylamine HCL and add it in methanol with sodium hudroxide it will becaome a solution?

jotoyNaOH converts the HCL in freebase like in any other process when basify or want to turns the HCL, sulphate...in freebase. Its nothing new.
Thanks.

 

[jotoy]

NaOH converts the HCL in freebase like in any other process when basify or want to turns the HCL, sulphate...in freebase. Its nothing new.
Thanks.

btcboss2022I tried to put noah to methylamine in methanol.while stirring slowly so doesnt overheat but still i can see a lot of crystals and it doesnt become a liquid solution

 

[jotoy]

I tried to put noah to methylamine in methanol.while stirring slowly so doesnt overheat but still i can see a lot of crystals and it doesnt become a liquid solution

jotoyNot the stirring slowly put i put noh slowly the stirring look strong enough

 

[hunter12]

Hi
Im a little confuse. So if i buy methylamine HCL and add it in methanol with sodium hudroxide it will becaome a solution?

jotoycompletely dissolved the methylamine hlc in methanol then add sodium hydroxide. salt will crush out and methylamine gas will dissolve in the methanol. You can filter out the salt or continue with the reaction (your choice)

 

[jotoy]

completely dissolved the methylamine hlc in methanol then add sodium hydroxide. salt will crush out and methylamine gas will dissolve in the methanol. You can filter out the salt or continue with the reaction (your choice)

hunter12So the trick is to find out how much methylamine have become solution
Let say: need 80 gramme of methylamine into mehtanol at a solution of 30%(80 g of methylamine+186.667g methanol =266.667g solution) but like all methylimine dosnt become solution because solid apears then how much methylamine to put more to keep it at 30 percent solution

 

[hunter12]

So the trick is to find out how much methylamine have become solution
Let say: need 80 gramme of methylamine into mehtanol at a solution of 30%(80 g of methylamine+186.667g methanol =266.667g solution) but like all methylimine dosnt become solution because solid apears then how much methylamine to put more to keep it at 30 percent solution

jotoyThe solids that appear is NaCl not methylmine hlc after adding NaOH. Water (H2O) and salt (NaCl) are produced as byproduct on this process so drying of the solution is essential for before you you continue with synthesis

 

[jotoy]

The solids that appear is NaCl not methylmine hlc after adding NaOH. Water (H2O) and salt (NaCl) are produced as byproduct on this process so drying of the solution is essential for before you you continue with synthesis

hunter12So my calculation is right but jusst before using it i need to dry with sulfate?

 

[hunter12]

So my calculation is right but jusst before using it i need to dry with sulfate?

jotoyYes you use MgSO4, silica gel, 3A molecular sieves or sodium sulfate to dry

 

[jotoy]

Yes you use MgSO4, silica gel, 3A molecular sieves or sodium sulfate to dry

hunter12IVe done that but something weird happen after to much solid stay after reaction and its very thick i e try to do around 33% methylamie solution in methanol

 

[mithyl2]

is there a viable way of doing this synth without a rotovap?

 

[sameoldstory]

Few Questions concerning BTCBOSS route for mdma - which if it works does seem quite promising but it does need a large reaction tank for 1kg batches!

1. Is a HDPE fermenter good enough as the vessel for this route - with a handy tap at the bottom

2. Would an airlock work on the top of this fermenter for any methylamine gas that may leak

3. does this reaction need to be sealed? - I am guessing so that's why the last question about the airlock or would it make sense to have a small rubber hose come out of the top of the reaction and then go outside?

4. would it be possible to just tap off the oil once the large amount of water has been added after the reaction and then do an acid/base with this oil and then washing and recrystallisation? - i think so from previous experiences but wouldnt mind others thoughts,

thanks in advance for any help