It looks like you have the process and all steps of the synthesis researched thoroughly. Here's my few notes:
- 500 ml acetone is too little for 250 g 2b4m. Have at least a liter, better 1.5 liters, available in your freezer. You may not need to use all but with 500 ml you would be rather short. Acetone used at this step can be recovered and reused again after a distillation.
- a magnetic stirrer/hot plate is an absolute must for consistency. It's the best $100 spent towards making 4-MMC .
- "drain ea ma layer which should be at the bottom" EA stays on top (it contains your free base), water that came from the MA aq 40 % is at the bottom. Drain water, like in all future washing steps.
- "does the flask need to be sealed or open here" always sealed, you can vent to release any pressure once done shaking
- your magnetic stirrer will not be able to work properly once the mixture thickens due to precipitated 4-MMC.HCl. Plan for this moment and have at least a spatula waiting, if not an overhead stirrer.
- dry acetone is acetone with as little water as possible. You should distill store-bought acetone to remove any contained water and impurities, but acetone purchased from trusted lab chemicals suppliers that is >99.5 % pure will work ok as well
- recrystallization does not require any other solvents than water, other solvents may speed up the process a little but they're costly so try and see how pure distilled water works for you. After some attempts with IPA and ethanol I don't use anything else anymore
- don't start with large (100 g or more) batches. Scale down the standard recipe to 1/4 and start with 25 g of BK4. That way you can confirm the process and everything works as you expect without wasting precious reagents before you get everything right. Once you confirm all is fine you scale up to 100 g batches or larger.
- By dodobird
How big a glass container would I need for say 250mg 2b4m
Assuming no mag stir hotplate is available, would love some alternates and details ...maybe shake will work just once for a demo until further funds are released ?
Do I need to grind the 2b4m and any easy way to tell if the one I have is good enough
Will probably have a white crystalline powder rather thank the cream yellow I see many using, is that okay
How can I get to salt stage easily within 6 hours or 8?
Something between conventional method and shakebake and Voss to Ave tone and labware
Does every stage need glassware
Assuming no mag stir hotplate is available, would love some alternates and details ...maybe shake will work just once for a demo until further funds are released ?
Do I need to grind the 2b4m and any easy way to tell if the one I have is good enough
Will probably have a white crystalline powder rather thank the cream yellow I see many using, is that okay
How can I get to salt stage easily within 6 hours or 8?
Something between conventional method and shakebake and Voss to Ave tone and labware
Does every stage need glassware
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I guessed based on your posts, no offense, we're all friends here.
Warm water will still work, but you may need to use more of it/do more washes to capture the same amount of methylamine that you would using cold water; and that will impact yield as more water will dissolve more EA and you'll lose some of the free base. If you can't get ice cold water which is strongly preferred then use warm, but understand the implications about lower yield.
Warm water will still work, but you may need to use more of it/do more washes to capture the same amount of methylamine that you would using cold water; and that will impact yield as more water will dissolve more EA and you'll lose some of the free base. If you can't get ice cold water which is strongly preferred then use warm, but understand the implications about lower yield.
