Full MDA Synthesis Starting from Helional
- Thread starter GhostChemist
- Start date
That's the "Two Dogs" method.
What's funny is that the hard part of this for me would be all the methylene chloride because it's no longer readily available for sale here because of it's toxicity. Can still get it, but now it's expensive and generates questions if bought in bulk.
I think I'd rather just reduce the oxime with sodium metal in anhydrous ethanol, and then take it from there.
What's funny is that the hard part of this for me would be all the methylene chloride because it's no longer readily available for sale here because of it's toxicity. Can still get it, but now it's expensive and generates questions if bought in bulk.
I think I'd rather just reduce the oxime with sodium metal in anhydrous ethanol, and then take it from there.
- By GhostChemist
Use another extragent such as toluene, petroleum ether, diethyl ether, chloroform etc.
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- By Field7
The "ethers" have distinct smells that I think it's best me to avoid.
Chloroform is a maybe... after all, making it uses bleach, too.
Toluene would be cool IF:
If used in the first step, it's not removed (or skip it and crystallization, but dry it etc and nice to step 2...
...use it as the solvent in step 2...
Here's the big "IF" though---
I know step 3 calls for the reaction in water... hear me out, please...
Could you leave the mixture in the toluene, and run it as a bi-phasic reaction?
In other words, your water and toluene layers go sloshing around together during step 3, and in the end, the toluene is separated, washed, acidified and separated from your now acidified aquas layer.
Because if it doesn't take part in the reaction in step 3 in any meaningful way), then you can just wash, dry, and move the toluene (and products) from step 1 through step 3, and then separate your product from it in the acid layer, and discard/recycle the toluene.
Sounds good to me for spitballing. Any thoughts from a peer?
Chloroform is a maybe... after all, making it uses bleach, too.
Toluene would be cool IF:
If used in the first step, it's not removed (or skip it and crystallization, but dry it etc and nice to step 2...
...use it as the solvent in step 2...
Here's the big "IF" though---
I know step 3 calls for the reaction in water... hear me out, please...
Could you leave the mixture in the toluene, and run it as a bi-phasic reaction?
In other words, your water and toluene layers go sloshing around together during step 3, and in the end, the toluene is separated, washed, acidified and separated from your now acidified aquas layer.
Because if it doesn't take part in the reaction in step 3 in any meaningful way), then you can just wash, dry, and move the toluene (and products) from step 1 through step 3, and then separate your product from it in the acid layer, and discard/recycle the toluene.
Sounds good to me for spitballing. Any thoughts from a peer?
- By GhostChemist
use filters for absorb the smells, any smells
in the first step my recomendation use extragent with low boiling point or decant oxime without extraction (if starting reagents are pure)
In the 2nd stage xylene is primary solvent with boiling point 140C
In the extraction of amine can be used chloroform and any other solvents
in the first step my recomendation use extragent with low boiling point or decant oxime without extraction (if starting reagents are pure)
In the 2nd stage xylene is primary solvent with boiling point 140C
In the extraction of amine can be used chloroform and any other solvents
- By Field7
The amine, ultimately, gets extracted with acidic H2O, and then that's evaporated to yield crude product
Spitballing Round #2.
1) Extract oxime from Step #1 with Xylene, wash it, dry it, use it in step #2.
2) Step #2 proceeds as illustrated, but final wash/rinse of solid amide done with butane instead.
3) Substitute DCM for Xylene.
My rationale? Here---
1) You're going to use Xylene in Step #2, so why not just extract with it at the end of Step #1? Right?
2) Why butane? Xylene will react with sodium hypochlorite so we need to remove what we can at the end of Step #2. It shouldn't dissolve, or react with, our amide. It's accessible, and has a super low BP.
But I'm hoping trace amounts of Xylene in Step #3 won't be a issue.
3) Why extract with Xylene towards the end of Step #3? Well... cause you already bought it. That's why.
Any peers think any left over Xylene would actually be an issue if along for the ride at the beginning of Step #3? Cause I'm kinda thinking it may actually assist the reaction by liberating some chlorine.
Don't say "Try it and let us know." Even though I probably will try it and let you, let's pretend, for now, that I didn't say it.
Spitballing Round #2.
1) Extract oxime from Step #1 with Xylene, wash it, dry it, use it in step #2.
2) Step #2 proceeds as illustrated, but final wash/rinse of solid amide done with butane instead.
3) Substitute DCM for Xylene.
My rationale? Here---
1) You're going to use Xylene in Step #2, so why not just extract with it at the end of Step #1? Right?
2) Why butane? Xylene will react with sodium hypochlorite so we need to remove what we can at the end of Step #2. It shouldn't dissolve, or react with, our amide. It's accessible, and has a super low BP.
But I'm hoping trace amounts of Xylene in Step #3 won't be a issue.
3) Why extract with Xylene towards the end of Step #3? Well... cause you already bought it. That's why.
Any peers think any left over Xylene would actually be an issue if along for the ride at the beginning of Step #3? Cause I'm kinda thinking it may actually assist the reaction by liberating some chlorine.
Don't say "Try it and let us know." Even though I probably will try it and let you, let's pretend, for now, that I didn't say it.
- By GhostChemist
Try it!
very interesting stage of "final wash/rinse of solid amide done with butane"
Butane - is a gas or liquid at -0.5C, and flammable if no ventilation hood in lab, this step is very danger
"2) Why butane? Xylene will react with sodium hypochlorite so we need to remove what we can at the end of Step #2. It shouldn't dissolve, or react with, our amide. It's accessible, and has a super low BP." What do you mean "Xylene will react with sodium hypochlorite"? Butane can react with sodium hypochlorite more than Xylene at UV and this stage carried out in water
very interesting stage of "final wash/rinse of solid amide done with butane"
Butane - is a gas or liquid at -0.5C, and flammable if no ventilation hood in lab, this step is very danger
"2) Why butane? Xylene will react with sodium hypochlorite so we need to remove what we can at the end of Step #2. It shouldn't dissolve, or react with, our amide. It's accessible, and has a super low BP." What do you mean "Xylene will react with sodium hypochlorite"? Butane can react with sodium hypochlorite more than Xylene at UV and this stage carried out in water
What would be an alternative DCM. It seems to be the only limiting factor.
Thanks a lot for this synthesis
Waiting for MDA HCL purification process video
Waiting for MDA HCL purification process video
I mean too much dcm use in this synthesis any alternative of dcm because this shit fucking cancer 
- By GhostChemist
DCM is the most popular solvent, but for extraction can be applied diethyl ether, petroleum ether etc.
Ethyl acetate in alkaline systems was destructed
Ethyl acetate in alkaline systems was destructed
The filtered solution is evaporated until crystallization. Fig 47
Temprature??
Temprature??
The resulting hydroxylamine solution is added to the helional solution over 20 hours. Fig 6
Fig 6
After adding all the hydroxylamine solution, the resulting RM is stirred for 20 hours yet. Fig 7
Fig 7
After 20 hours, a solid oxime may form. Fig 8
My question is how much time take to add hydroxylamine 20 hours and 20 hour 20+20
I mean can I do 40 hour RM stirre or just 20 hour ?
40 hours is loot
Fig 6
After adding all the hydroxylamine solution, the resulting RM is stirred for 20 hours yet. Fig 7
Fig 7
After 20 hours, a solid oxime may form. Fig 8
My question is how much time take to add hydroxylamine 20 hours and 20 hour 20+20
I mean can I do 40 hour RM stirre or just 20 hour ?
40 hours is loot