Today I will be updating my old rushed synthesis of the shake and bake. This will include proper glassware, equipment, washing of impurities, and recrystallization with additional purifications like cold anhydrous acetone washings!
Precursors needed with measurements:
10 grams of ephedrine or pseudoephedrine
Full Lithium Metal strip from AA energizer lithium batterys (STORE IN MINERAL OIL OR YOUR NON POLAR SOLVENT YOU ARE GOING TO USE, non polar solvent if you already have your reaction mixture and your about to add your lithium after peeling)
Ammonium Nitrate 30 - 40 grams for sufficient ammonia gas production to react with lithium (35 grams would be sufficient)
Sodium Hydroxide 15 - 20 grams to fully react with the ammonium nitrate and to freebase the 10 grams of ephedrine and or pseudoephedrine (20 grams is recommended)
Toluene 100 - 200ml (150mls would work fine in the 1000ml flat bottom boiling flask)
Distilled Water 4ml to start the reaction
Equipment needed and other chemicals:
1000ml flat bottom boiling flask
a pot bigger than the flask that you will fill with ice
ice
pliers to strip the battery
rubber stopper with a small hole to place on the flask
250ml beaker 3x
500ml beaker 2x
sulfuric acid 98% from walmart or a chemical supplier 10ml
Table salt 5 - 10 grams
plastic water bottle with a vinyl tube to go through the bottle cap when gassing freebase
coffee filters
plastic funnel
vinyl tubing as previously mentioned
anhydrous isopropyl alcohol 99% 50ml (for recrystallization)
anhydrous acetone 5ml (to add to the isopropanol)
anhydrous acetone 10ml (for the washing after precipitation of hydrochloride salt)
anhydrous magnesium sulfate 5grams
Ph Strips to see what the Ph is
The Reaction:
in a 1000ml flat bottom boiling flask add 10 grams of grinded up ephedrine or pseudoephedrine make sure its a fine powder, to this you add 35 grams of ammonium nitrate the ratios should be 3:1 - 4:1 of ammonium nitrate to pseudoephedrine by weight.
add your toluene 150ml then in a 250ml beaker add 100ml toluene and dip the whole strip of lithium in to prevent oxidation then proceed to tear it into small pieces adding it to the flask once finished get a pot that is bigger than the flask and fill with ice
place the flask into the ice filled pot and pour salt on the ice to reduce temperature further as you do not want it to overheat and cause a runaway reaction or byproduct formation. Once the lithium has been added get your 20 grams of sodium hydroxide and add to the flask slowly
once added get 4ml of cooled distilled water and add to the flask but do so quickly as this will start the reaction and it will violently boil and release ammonia gas. once added place your stopper with a hole on the flask and swirl for 8 seconds. once its violently boiling and reacting
keep it in the ice bath and let it sit, do NOT leave this reaction without monitoring it. after you have swirled and its violently boiling wait about 2 minutes before swirling again to keep mixing reactants, after 2 minutes you should see the formation of these bronze bubbles coming from the lithium metal
these are Solvated Electrons this is a very good sign the reduction is proceeding smoothly. if you notice the solid reagents you have added are stuck to the bottom then make sure to swirl more but no too vigourously as to not interrupt the formation of these electrons.
keep repeating these steps and keep the rubber stopper on
the small hole in the stopper is to not build up pressure and have the flask explode or crack, that would be a pretty awful scenario in itself. if the reaction ceases quickly than you can GENTLY heat it to kick start the reaction again or you can add a bit more sodium hydroxide about 2 - 5 grams should suffice but make sure to add every 20 minutes if needed
after about 2 - 3 hours the reaction should be complete when bubbling ceases and no visual reaction taking place.
Filtering and Drying:
take the stopper off carefully and put on a respirator with goggles because ammonia will spew out but you wont see it. It WILL burn your eyes and throat causing you to feel like your suffocating, as someone whos taken large whiffs of ammonia gas unwillingly...trust me i know...
get your 500ml beaker and place a plastic funnel on it with 2 coffee filters then after filtering wait until the ammonia smell is gone and then proceed to dry the liquid with anhydrous magnesium sulfate 5grams and cover the beaker with saram wrap and swirl for 1 minute then let it sit for 30 minutes
this should leave you with a clear freebase of your methamphetamine.
Precipitation of Methamphetamine Hydrochloride:
After you have dried your freebase grab the other 500ml beaker and decant your methamphetamine freebase from the hydrated magnesium sulfate then in the new beaker with your freebase wrap with saram wrap and leave an opening near where you pour liquids out the beaker to fit the tube through, grab your water bottle and pour in about 5grams of regular table salt u get from the store and pour in 10ml of sulfuric acid but before adding the sulfuric acid make sure you have your tube inside the water bottle cap
so your ready to gas your product, under a fume hood or wearing a respirator or simply hold your breath pour in 10ml of the 98% sulfuric acid into the bottle and screw on the water bottle cap with the tube and place the tube where the opening of the beaker covered with saram wrap is at. proceed to gas the freebase until you reach a ph of 3 and all your product should precipitate out as a salt. This is methamphetamine hydrochloride.
once youve achieved a ph of 3 or 3.5 cover the opening of the beaker with the saram wrap you peeled back and secure it with a rubber band and place in the freezer for 2 hours to decrease methamphetamine solubility and fully precipitate out. once thats done get another 250ml beaker and place your plastic funnel in it and with 2 fresh new coffee filters filter your methamphetamine hydrochloride then place in a pyrex dish to dry with a fan on. monitor it until you see its fully dry.
Acetone Wash:
Now that you have your dried methamphetamine hydrochloride place it inside of a beaker or mason jar. Take your bottle of anhydrous acetone and place in the fridge for 30 minutes to and hour or until its nice and cold then pour 10ml of it over your methamphetamine hydrochloride and swirl or use a glass stirrod to mix around, once finished decant into another beaker and repeat this process 2 to 3 more times and it will leave you with a nice and pure crystalline salt! make sure to let it dry after the final wash and decantation.
Recrystallization:
Now that you have relatively pure methamphetamine if you want those nice shards you can recrystallize. Place your clean methamphetamine hydrochloride in a beaker and add 50ml of 99% isopropyl alcohol and heat until boiling but while heating wrap it with saram wrap or place a watch glass on top of it to prevent excessive evaporation and loss of product. stir until fully dissolved then take off heating and add 5ml of room temperature anhydrous acetone and let it cool to room temperature then in a pyrex crystallization dish let it evaporate slowly at room temperature or in the freezer.
this can take a few hours to a few days. once you have your nice and dry shards of methamphetamine you can wash with acetone or proceed to use it.
Conclusion:
This is my personal method and techniques i take to purify my methamphetamine to very high puritys of up to 95 - 99 percent pure. ive had a lot of success doing so and good results! Remember to be careful and USE YOUR BRAIN. Good cooking.
Precursors needed with measurements:
10 grams of ephedrine or pseudoephedrine
Full Lithium Metal strip from AA energizer lithium batterys (STORE IN MINERAL OIL OR YOUR NON POLAR SOLVENT YOU ARE GOING TO USE, non polar solvent if you already have your reaction mixture and your about to add your lithium after peeling)
Ammonium Nitrate 30 - 40 grams for sufficient ammonia gas production to react with lithium (35 grams would be sufficient)
Sodium Hydroxide 15 - 20 grams to fully react with the ammonium nitrate and to freebase the 10 grams of ephedrine and or pseudoephedrine (20 grams is recommended)
Toluene 100 - 200ml (150mls would work fine in the 1000ml flat bottom boiling flask)
Distilled Water 4ml to start the reaction
Equipment needed and other chemicals:
1000ml flat bottom boiling flask
a pot bigger than the flask that you will fill with ice
ice
pliers to strip the battery
rubber stopper with a small hole to place on the flask
250ml beaker 3x
500ml beaker 2x
sulfuric acid 98% from walmart or a chemical supplier 10ml
Table salt 5 - 10 grams
plastic water bottle with a vinyl tube to go through the bottle cap when gassing freebase
coffee filters
plastic funnel
vinyl tubing as previously mentioned
anhydrous isopropyl alcohol 99% 50ml (for recrystallization)
anhydrous acetone 5ml (to add to the isopropanol)
anhydrous acetone 10ml (for the washing after precipitation of hydrochloride salt)
anhydrous magnesium sulfate 5grams
Ph Strips to see what the Ph is
The Reaction:
in a 1000ml flat bottom boiling flask add 10 grams of grinded up ephedrine or pseudoephedrine make sure its a fine powder, to this you add 35 grams of ammonium nitrate the ratios should be 3:1 - 4:1 of ammonium nitrate to pseudoephedrine by weight.
add your toluene 150ml then in a 250ml beaker add 100ml toluene and dip the whole strip of lithium in to prevent oxidation then proceed to tear it into small pieces adding it to the flask once finished get a pot that is bigger than the flask and fill with ice
place the flask into the ice filled pot and pour salt on the ice to reduce temperature further as you do not want it to overheat and cause a runaway reaction or byproduct formation. Once the lithium has been added get your 20 grams of sodium hydroxide and add to the flask slowly
once added get 4ml of cooled distilled water and add to the flask but do so quickly as this will start the reaction and it will violently boil and release ammonia gas. once added place your stopper with a hole on the flask and swirl for 8 seconds. once its violently boiling and reacting
keep it in the ice bath and let it sit, do NOT leave this reaction without monitoring it. after you have swirled and its violently boiling wait about 2 minutes before swirling again to keep mixing reactants, after 2 minutes you should see the formation of these bronze bubbles coming from the lithium metal
these are Solvated Electrons this is a very good sign the reduction is proceeding smoothly. if you notice the solid reagents you have added are stuck to the bottom then make sure to swirl more but no too vigourously as to not interrupt the formation of these electrons.
keep repeating these steps and keep the rubber stopper on
the small hole in the stopper is to not build up pressure and have the flask explode or crack, that would be a pretty awful scenario in itself. if the reaction ceases quickly than you can GENTLY heat it to kick start the reaction again or you can add a bit more sodium hydroxide about 2 - 5 grams should suffice but make sure to add every 20 minutes if needed
after about 2 - 3 hours the reaction should be complete when bubbling ceases and no visual reaction taking place.
Filtering and Drying:
take the stopper off carefully and put on a respirator with goggles because ammonia will spew out but you wont see it. It WILL burn your eyes and throat causing you to feel like your suffocating, as someone whos taken large whiffs of ammonia gas unwillingly...trust me i know...
get your 500ml beaker and place a plastic funnel on it with 2 coffee filters then after filtering wait until the ammonia smell is gone and then proceed to dry the liquid with anhydrous magnesium sulfate 5grams and cover the beaker with saram wrap and swirl for 1 minute then let it sit for 30 minutes
this should leave you with a clear freebase of your methamphetamine.
Precipitation of Methamphetamine Hydrochloride:
After you have dried your freebase grab the other 500ml beaker and decant your methamphetamine freebase from the hydrated magnesium sulfate then in the new beaker with your freebase wrap with saram wrap and leave an opening near where you pour liquids out the beaker to fit the tube through, grab your water bottle and pour in about 5grams of regular table salt u get from the store and pour in 10ml of sulfuric acid but before adding the sulfuric acid make sure you have your tube inside the water bottle cap
so your ready to gas your product, under a fume hood or wearing a respirator or simply hold your breath pour in 10ml of the 98% sulfuric acid into the bottle and screw on the water bottle cap with the tube and place the tube where the opening of the beaker covered with saram wrap is at. proceed to gas the freebase until you reach a ph of 3 and all your product should precipitate out as a salt. This is methamphetamine hydrochloride.
once youve achieved a ph of 3 or 3.5 cover the opening of the beaker with the saram wrap you peeled back and secure it with a rubber band and place in the freezer for 2 hours to decrease methamphetamine solubility and fully precipitate out. once thats done get another 250ml beaker and place your plastic funnel in it and with 2 fresh new coffee filters filter your methamphetamine hydrochloride then place in a pyrex dish to dry with a fan on. monitor it until you see its fully dry.
Acetone Wash:
Now that you have your dried methamphetamine hydrochloride place it inside of a beaker or mason jar. Take your bottle of anhydrous acetone and place in the fridge for 30 minutes to and hour or until its nice and cold then pour 10ml of it over your methamphetamine hydrochloride and swirl or use a glass stirrod to mix around, once finished decant into another beaker and repeat this process 2 to 3 more times and it will leave you with a nice and pure crystalline salt! make sure to let it dry after the final wash and decantation.
Recrystallization:
Now that you have relatively pure methamphetamine if you want those nice shards you can recrystallize. Place your clean methamphetamine hydrochloride in a beaker and add 50ml of 99% isopropyl alcohol and heat until boiling but while heating wrap it with saram wrap or place a watch glass on top of it to prevent excessive evaporation and loss of product. stir until fully dissolved then take off heating and add 5ml of room temperature anhydrous acetone and let it cool to room temperature then in a pyrex crystallization dish let it evaporate slowly at room temperature or in the freezer.
this can take a few hours to a few days. once you have your nice and dry shards of methamphetamine you can wash with acetone or proceed to use it.
Conclusion:
This is my personal method and techniques i take to purify my methamphetamine to very high puritys of up to 95 - 99 percent pure. ive had a lot of success doing so and good results! Remember to be careful and USE YOUR BRAIN. Good cooking.