Full MDA Synthesis Starting from Helional

[Field7]

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.

 

[GhostChemist]

Use another extragent such as toluene, petroleum ether, diethyl ether, chloroform etc.

 

[Field7]

Yeah. But the idea is to rinse the solid product to remove some Xylene. Any remaining butane will evaporate quickly.

But again--- that little bit of Xylene may actually help the reaction along.

It's a toss up.

I think I'll try it without the butane rinse, first. It's less work, and if it goes well, then great.

I'll try that in the near future. Yes-- I'll share the results. 'Cause it's not just me that wants to avoid DCM.

 

[Field7]

I get that, but again--- I'm talking about what I think would be a small amount left over from the previous reaction.

Trying to avoid DCM and streamline the process.

 

[smoozzi]

I can use CH3OH? I dont have EtOh

 

[goku1008]

Can I replace dcm in stage 1 and 2 with ethyl acetate ? Plz answer

 

[GhostChemist]

Yes

 

[bodek87]

Is 98% pure helional will be good for this reaction?

 

[GhostChemist]

yep

 

[chmclngr]

When is the remaining o-Xylene suppposed to be added after figure 18, where 200mL is added? Im asssuming shortly after, perhaps after adding the Nickel Acetate?

 

[GhostChemist]

Have you watched the video?

http://bbzzzsvqcrqtki6umym6itiixfhn...yd.onion/media/mda-synthesis-part-2-of-3.124/

 

[chmclngr]

I missed it. Thanks.

 

[4mmc1]

sodium hypochlorite how much % ?

 

[chmclngr]

13.5%

 

[GhostChemist]

See Figure 36

 

[4mmc1]

70% of amide it means almost 105g mda I'm i right ?

 

[GhostChemist]

approximately yes (105-109 g)

 

[Tippingpointover]

If switching to toluene, would any adjustments have to be made? Or can you stick to the same recipe, just switching out toluene for dcm? Thanks

 

[GhostChemist]

Is the toluene will be used in the process of extraction?

 

[Rox2]

You can use toluene besides xylene in step 2, recristallize amide from toluene too . And in step 3 use tol for extraction of amine.

 

[Rox2]

Yes it can be used very efficiently and in step 2 besides xilol too and for recriztallization of amide

 

[4mmc1]

Can I also use toluene in stage 3 mda stage

 

[Rox2]

Yes You can

 

[Rox2]