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If you. Can spot any issues, or add anything to it would be greatly appreciated. I'm going to try to do a series of videos. To contribute to the forum and do a giveaway of product so I want it to contain as much info as possible and the product to be semi decent for consumption.
Feel.free to maybe advise a tweet or trick that helps you out and I will Include it. Knowledge is power people let's spread it.
Phase 1. (100g bk4 + 300ml DCM)
Dissolve 2b4mp in dichloromethane (DCM) in a reactor / flat bottom round flask.
(warm it slightly to help dilution 25ºC)
Phase 2 and 3 (200-ML of MA 40%)
Add a 40% aqueous solution of methylamine in batches so that the temperature does not rise above 40ºC. 50 ml every 5 minutes. ( total 30 min) DO NOT CROSS 40ºC
[methylamine addition causes exothermic reaction]
Phase 3 (do not cross 40ºC)
Keep mixing solution for 4 hrs at ~35ºC.
Turn on the heat as soon as the temperature begins to drop.
AFTER 4 hours transfer to glass beaker.
GLASS BEAKER on stirrer
Phase 4.
FIRST WASH: Add 500 ml 5% sodium bicarbonate solution around 30ºC
(Separate the layers as much as possible with overhead stirrer)
TRANSFER to Separation funnel.
let sit 60 min (drain bottom layer)
GLASS BEAKER / stirrer / mixer
2nd wash 200 ml demi water at 30ºC
Stir well for about 10 minutes.
Transfer to separation funnel
SEPERATION FUNNEL.
Let sit 4MMC solution sit for 30 min
If a bit cloudy add a dash of sodium bicarbonate shake in separation funnel and let sit for 30 minutes. Drain bottom water layer. Transfer to Glass Beaker.
GLASS BEAKER
Phase 5 (150ml Acetone + 30ml HCL)
Add ICE COLD acidification mixture drip by drip into it 4mmc solution while magnetic stirrer is on a high setting. Keep checking ph levels. When PH level reach 5 stop and transfer to a plastic beaker. Set in fridge for 10 hours.
( you do not have use all your solution, only the PH level is important)
GLASS BEAKER small ( quality check)
Phase 6.
Grind 4mmc solid to powder
Take 1 gram of powder and disolve in demi water at 90 ºC
Now we can see the solution colour.
The darker the colour the more impurities are present. We want to see a clear solution. If not clear we need extra purification. ( atleast darker than the colour of a lemon)
Vaccum filter.
BUCHNER FUNNEL / Glass spatula
Phase 7. (Ice cold acetone)
Place crushed powder into funnel and first use a small bit of cold IPA, after that wash in acetone all while gently stirring the 4mmc on the filter paper. Allow the IPA and Acetone to evaporate before applyimg more so the 4mmc dosent Dissolve into the alcohol.
Make sure the powder is more of a free moving thick liquid consistency. If it is clay like it can clog the filter paper.
Leave the vaccum running for a bit untill you have a dry consistency.
Transfer the powder to a dish and use a infrared light to finish the drying, in a warm dry room.
It's ready when it has a powdery refractive look.
DO NOT THROW WASTE LIQUID
YIELD.
If your overall weight has lost a large % of mass its possible 4MMC is still in the IPA and acetone. Allow more than 50% of the liquid to evaporate slowly, and run it through. The filter again
CRYSTALLISATION (optional)
GLASS BEAKER / heated mixer.
(1g to 1ml Demi water/1ml IPA)
Mix your 4mmc into your solution heat to around 80ºC (very small bubbles) all while running your magnetic mixer vigorously.
CRYSTALLISATION DISH
(Pyrex can take heat and cold)
phase 9.
Pour the 4 mmc solution into dish
Preferably leave to crystallize in a dry room at 18-20ºC. It is preferable to use an air conditioner. When crystallization stops put into the freezer for 8 hours
The more water you use, the larger the crystals and the longer it will take once done remove crystals from dish
Wash crystals with ice cold acetone in Buchner funnel, once or twice.
Feel.free to maybe advise a tweet or trick that helps you out and I will Include it. Knowledge is power people let's spread it.
Phase 1. (100g bk4 + 300ml DCM)
Dissolve 2b4mp in dichloromethane (DCM) in a reactor / flat bottom round flask.
(warm it slightly to help dilution 25ºC)
Phase 2 and 3 (200-ML of MA 40%)
Add a 40% aqueous solution of methylamine in batches so that the temperature does not rise above 40ºC. 50 ml every 5 minutes. ( total 30 min) DO NOT CROSS 40ºC
[methylamine addition causes exothermic reaction]
Phase 3 (do not cross 40ºC)
Keep mixing solution for 4 hrs at ~35ºC.
Turn on the heat as soon as the temperature begins to drop.
AFTER 4 hours transfer to glass beaker.
GLASS BEAKER on stirrer
Phase 4.
FIRST WASH: Add 500 ml 5% sodium bicarbonate solution around 30ºC
(Separate the layers as much as possible with overhead stirrer)
TRANSFER to Separation funnel.
let sit 60 min (drain bottom layer)
GLASS BEAKER / stirrer / mixer
2nd wash 200 ml demi water at 30ºC
Stir well for about 10 minutes.
Transfer to separation funnel
SEPERATION FUNNEL.
Let sit 4MMC solution sit for 30 min
If a bit cloudy add a dash of sodium bicarbonate shake in separation funnel and let sit for 30 minutes. Drain bottom water layer. Transfer to Glass Beaker.
GLASS BEAKER
Phase 5 (150ml Acetone + 30ml HCL)
Add ICE COLD acidification mixture drip by drip into it 4mmc solution while magnetic stirrer is on a high setting. Keep checking ph levels. When PH level reach 5 stop and transfer to a plastic beaker. Set in fridge for 10 hours.
( you do not have use all your solution, only the PH level is important)
GLASS BEAKER small ( quality check)
Phase 6.
Grind 4mmc solid to powder
Take 1 gram of powder and disolve in demi water at 90 ºC
Now we can see the solution colour.
The darker the colour the more impurities are present. We want to see a clear solution. If not clear we need extra purification. ( atleast darker than the colour of a lemon)
Vaccum filter.
BUCHNER FUNNEL / Glass spatula
Phase 7. (Ice cold acetone)
Place crushed powder into funnel and first use a small bit of cold IPA, after that wash in acetone all while gently stirring the 4mmc on the filter paper. Allow the IPA and Acetone to evaporate before applyimg more so the 4mmc dosent Dissolve into the alcohol.
Make sure the powder is more of a free moving thick liquid consistency. If it is clay like it can clog the filter paper.
Leave the vaccum running for a bit untill you have a dry consistency.
Transfer the powder to a dish and use a infrared light to finish the drying, in a warm dry room.
It's ready when it has a powdery refractive look.
DO NOT THROW WASTE LIQUID
YIELD.
If your overall weight has lost a large % of mass its possible 4MMC is still in the IPA and acetone. Allow more than 50% of the liquid to evaporate slowly, and run it through. The filter again
CRYSTALLISATION (optional)
GLASS BEAKER / heated mixer.
(1g to 1ml Demi water/1ml IPA)
Mix your 4mmc into your solution heat to around 80ºC (very small bubbles) all while running your magnetic mixer vigorously.
CRYSTALLISATION DISH
(Pyrex can take heat and cold)
phase 9.
Pour the 4 mmc solution into dish
Preferably leave to crystallize in a dry room at 18-20ºC. It is preferable to use an air conditioner. When crystallization stops put into the freezer for 8 hours
The more water you use, the larger the crystals and the longer it will take once done remove crystals from dish
Wash crystals with ice cold acetone in Buchner funnel, once or twice.