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]

Da. Dar ideea este de a clăti produsul solid pentru a elimina o parte din xilen. Orice butan rămas se va evapora rapid.

Dar, din nou, acel pic de xilen poate ajuta de fapt reacția.

Este o incertitudine.

Cred că voi încerca mai întâi fără clătirea cu butan. E mai puțină muncă, iar dacă merge bine, atunci minunat.

Voi încerca asta în viitorul apropiat. Da - voi împărtăși rezultatele. Pentru că nu doar eu vreau să evit DCM.

 

[Field7]

Înțeleg, dar din nou - vorbesc despre ceea ce cred că ar fi o cantitate mică rămasă de la reacția anterioară.

Încerc să evit DCM și să simplific procesul.

 

[smoozzi]

Pot utiliza CH3OH? Nu am 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]