meth crystalization from ephedrine to ice cant be done

[evangelium]

Hello im trying to make hard nice shards by way of dissolving meth in ethanol and when its completly dissolved it should be heated up to 180°. But that wasnt sucesfull it allways stopped at 80° whete js the ethanol boiling point. Is possible to go beyond boiling point ?
Anyway in the 80° i tryed to put glass rod in to it and took it out and wait if it will crystaline. It did so i let it cool on room temperature where it started to look nice and after cooling to room temperature i put it in freezer for 7 hours but the crystals arnt as they should look like

What did i do wrong ?
Whats the solution ?
Is the method im using sutable ?

Thanks for all help

 

[23rdgate]

Try boiling under vacuum to lower the boil point

 

[evangelium]

Try boiling under vacuum to lower the boil point

23rdgateHow can i do that

 

[23rdgate]

Flat bottom vertical condenser into gas bubbler

 

[Frit Buchner]

The problem here is there is not enough alcohol left in the pan for crystalization to occur. You basically just evaporated the solvent off. You need a pyrex beaker or flask vand you need to heat your alcohol in a separate container. Have the meth in 1 beaker dry and your alcohol in another container, cbith on the same heat source. When the alcohol starts boiling pour some into the eth and swirl it. Put them both back on the heat. Add more boiling alcohol until all of the meth is dissolved tae it off f the heat and just leave it set still for 12: hours. N heat no breeze no vibration. Nothing. Then out it in the fridge for 8 hours then the freezer. It has to cool slowly to make big crystals should probably wrap a dish towel around it until it goes in the fridge. Letting it cool slowly is the key and it has to have enough alcohol that it doesn't over saturated and precipitate. Some anhydrous acetone would help, a daily solvent crystalization. Vacuum won't help in any way I can imagine and no one has ever done that that I've seen

 

[evangelium]

The problem here is there is not enough alcohol left in the pan for crystalization to occur. You basically just evaporated the solvent off. You need a pyrex beaker or flask vand you need to heat your alcohol in a separate container. Have the meth in 1 beaker dry and your alcohol in another container, cbith on the same heat source. When the alcohol starts boiling pour some into the eth and swirl it. Put them both back on the heat. Add more boiling alcohol until all of the meth is dissolved tae it off f the heat and just leave it set still for 12: hours. N heat no breeze no vibration. Nothing. Then out it in the fridge for 8 hours then the freezer. It has to cool slowly to make big crystals should probably wrap a dish towel around it until it goes in the fridge. Letting it cool slowly is the key and it has to have enough alcohol that it doesn't over saturated and precipitate. Some anhydrous acetone would help, a daily solvent crystalization. Vacuum won't help in any way I can imagine and no one has ever done that that I've seen

Frit BuchnerThank you ! I recrystalized it and cool it down slowly and now its looking much better but i didnt had it separated it good think to know

 

[Frit Buchner]

Ethanols boiling point is 178°f /78°C. You could raise it in a pressure cooker but probably only to 210°f without modification to the PC to go higher than 15 psi