You can scale it proportionally (in large amounts methylamine may be added in more parts)
Reagents:
1. 2b4m 100g;
2. Ethyl Acetate 500ml;
3. Distilled water ~2l;
4. NaOH 100g;
5. Methylamine HCL 150g;
6. Acetone 500-1000ml;
7. HCL acid 50-70 ml;
Equipment:
1. Magnetic stirrer;
2. Beaker 200ml (can be any volume) and 1000 ml (wide);
3. Flask;
4. Scale;
5. Mechanical stirrer (can use cordless drill);
6. thermometer;
7. Dish for water bath;
8. Separation funnel;
9. Buchner funnel;
10. Vacuum pump;
1.Dissolve 100g NaOH in 200 ml H2O. Stir it until its dissolved on magnetic stirrer, then let it chill for about 1h, temperature should be as close to room temp.
2.Grind 2b4m and add it into 500ml ethyl acetate in flask on magnetic stirrer.
3. After 2b4m is dissolved, put dish with cold water, to provide cooling to flask
4. Prepare Methylamine HCL 150g to be poured into flask instantly after adding NaOH + H2O solution (1st put NaOH into flask, then Methylamine HCL)
5. Add NaOH + H2O solution into flask
6. Add methylamine HCL into flask (make sure that your magnetic stirrer is capable to stir it, otherwise you will need mechanical one - on my magnetic stirrer it was necesarry to add methylamine in 2 parts so it could constantly stir, if you don't use water bath you need to check for temperature rinse and add methylamine in 2-3 parts because temp can go too hot, for larger scale its recommended to monitor temperature and add methylamine into parts).
7. After temperature starts to rinse, stir it for 30 mins. The reaction temp when using 1°C water bath was about 30°C.
8. after reaction is complete, pour mixture into buchner funnel and separate freebase from solid compounds that are left.
9. Sodium bicarbonate 5% H2O solution 300 ml was poured into flask with freebase then stirred for 30 mins. After that layers are separated clearly
10. Mixture is poured into separation funnel. 3 times rinsing with 300 ml cold H2O is done. (ofc bottom layer is to be discarded - top layer is organic one to keep to futher work, allow at least 5 mins between washes to separate layers properly).
11. After rinsing, mixture is transfered into beaker 1000ml, ice cold acetone is added in amount 1:1 of remaining freebase
12. HCL acid is added into separation funnel
13. Mechanical stirrer is turned on
14. HCL acid is slowly dropping on rate 1 drop per 1s
15. PH must be measured, you should close the valve to see ph, then if its not 5 yet open valve again.
You should receive full white solution, use film to make it close, put it into freezer for 12h.
after 12h take it out, transfer into buchner funnel and turn on vacuum pump
addictional purification is no needed, product should be full white.
Let the pump work for 30 mins after whole liquid is in the flask, then it will need some hours to be dried.
Prepare crystalization.
For start use 1:1 1ml water per 1g of product in powder. Simply heat it to boiling and dissolve product. Let it be hot at 90c and wait until "shard" in the top of mixture start to be visable. Mixtgure becomes saturated. To heating use water bath that should be left on flask. It will slowly cool down. When its room temp put it into fridge 10 celcius degree, then after 1h put it into fridge 1 celcius degree. You can use water with ice to slowly decrashe temp from room temp to 1celcius degree.
After its 1 celcious degree, transfer it on buchner funnel, take rest of liquid to beaker and leave it to futher crystalization or heat it again to make oversaturated solution to crystalize again.
The yield is 62.5% (75 g) from 120 g 2B4M.
Reagents:
1. 2b4m 100g;
2. Ethyl Acetate 500ml;
3. Distilled water ~2l;
4. NaOH 100g;
5. Methylamine HCL 150g;
6. Acetone 500-1000ml;
7. HCL acid 50-70 ml;
Equipment:
1. Magnetic stirrer;
2. Beaker 200ml (can be any volume) and 1000 ml (wide);
3. Flask;
4. Scale;
5. Mechanical stirrer (can use cordless drill);
6. thermometer;
7. Dish for water bath;
8. Separation funnel;
9. Buchner funnel;
10. Vacuum pump;
1.Dissolve 100g NaOH in 200 ml H2O. Stir it until its dissolved on magnetic stirrer, then let it chill for about 1h, temperature should be as close to room temp.
2.Grind 2b4m and add it into 500ml ethyl acetate in flask on magnetic stirrer.
3. After 2b4m is dissolved, put dish with cold water, to provide cooling to flask
4. Prepare Methylamine HCL 150g to be poured into flask instantly after adding NaOH + H2O solution (1st put NaOH into flask, then Methylamine HCL)
5. Add NaOH + H2O solution into flask
6. Add methylamine HCL into flask (make sure that your magnetic stirrer is capable to stir it, otherwise you will need mechanical one - on my magnetic stirrer it was necesarry to add methylamine in 2 parts so it could constantly stir, if you don't use water bath you need to check for temperature rinse and add methylamine in 2-3 parts because temp can go too hot, for larger scale its recommended to monitor temperature and add methylamine into parts).
7. After temperature starts to rinse, stir it for 30 mins. The reaction temp when using 1°C water bath was about 30°C.
8. after reaction is complete, pour mixture into buchner funnel and separate freebase from solid compounds that are left.
9. Sodium bicarbonate 5% H2O solution 300 ml was poured into flask with freebase then stirred for 30 mins. After that layers are separated clearly
10. Mixture is poured into separation funnel. 3 times rinsing with 300 ml cold H2O is done. (ofc bottom layer is to be discarded - top layer is organic one to keep to futher work, allow at least 5 mins between washes to separate layers properly).
11. After rinsing, mixture is transfered into beaker 1000ml, ice cold acetone is added in amount 1:1 of remaining freebase
12. HCL acid is added into separation funnel
13. Mechanical stirrer is turned on
14. HCL acid is slowly dropping on rate 1 drop per 1s
15. PH must be measured, you should close the valve to see ph, then if its not 5 yet open valve again.
You should receive full white solution, use film to make it close, put it into freezer for 12h.
after 12h take it out, transfer into buchner funnel and turn on vacuum pump
addictional purification is no needed, product should be full white.
Let the pump work for 30 mins after whole liquid is in the flask, then it will need some hours to be dried.
Prepare crystalization.
For start use 1:1 1ml water per 1g of product in powder. Simply heat it to boiling and dissolve product. Let it be hot at 90c and wait until "shard" in the top of mixture start to be visable. Mixtgure becomes saturated. To heating use water bath that should be left on flask. It will slowly cool down. When its room temp put it into fridge 10 celcius degree, then after 1h put it into fridge 1 celcius degree. You can use water with ice to slowly decrashe temp from room temp to 1celcius degree.
After its 1 celcious degree, transfer it on buchner funnel, take rest of liquid to beaker and leave it to futher crystalization or heat it again to make oversaturated solution to crystalize again.
The yield is 62.5% (75 g) from 120 g 2B4M.
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a lot of things may go wrong.
