Breaks in the process

[SuperStar]

SWIM is going this path to MDMA.
1. Safrole
2. Iso
3. Oxone
4. MM
5. Gas (no recrystal)

The problem is SWIM needs it broken up a little bit more. Seems like the Oxone followed by the H2S04 is too long time wise for one run with SWIM. 

Question1: After removing the DCM from the post Oxone reaction what would be the proper techniques to store the glycol oil before doing the H2S04 rearrangement. How long? Temp? light?

Question2: After the MM AL reaction and after the extraction and washings. How long can product sit in Toulene? Freezer?  light problems?  Say you were not going to dry the toulene and gas until the next day.

Question 3: Need some experienced estimates on how many hours to go from starting MM AL to finished with washed toulene?  Would 7 hours be enough time?

SWIM thinks these 2 breaks along with the natural breaks will be enough.
Pardon my friend officer, He's a little slow.

[pickler]

Time is money, but that's your personal choice. Swim does the oxone method and mm so he might be able to help.
1.Distill a lot of safrole and have handy so you don't have to distill it everytime.
2.Make all safrole into isosafrole and store properly.
   doing these two above steps will save tons of time for starters.
3.Make sure to filter your oxone before adding your iso to it. Cuts out the the vacuum filtering step. You could even just tap off the epoxide mixture if you really want and save some time. Tapping off the epoxide mixture would cut out the dcm distillation.
4. For the h2so4, make a gallon of it and have it ready to use. Saves a lot of time.Again you could just tap off the ketone at the end and save some time.
   Tapping off the ketone or epoxide will lower yields, but will save time.
4. To save time with the MM synth, have lots of al cut and weighed out in baggies ready.

Question 1- Swim has no idea on storage time of epoxide, freezer sounds right in glass container. Swim has left epoxide out in flask for 2 days with no probs.

question 2- If you made it that far, you only have about 2hrs left. Sorry, always finished from that point. Swim thinks there was some threads on that. try the search engine.

Question 3- MM takes 5hrs to run it and the rest depends on you. The more comfortable you are in the lab, the better things go. & hrs seems about right though.
We'll soon find out if I'm a chemist or not!

[SuperStar]

Thanks Pick. Right now SWIM not too concerned with yields, just getting active product that is clean.  SWIM will try skipping the DCM extracts. That seems like would save lot's of time not only setting up but cleaning and drying dishes. SWIM can't leave stuff setup must assemble and deassemble everytime.
Pardon my friend officer, He's a little slow.

[pickler]

Swim only has so many hours per day to do stuff. If swim can cut out a few hours here and there, to hell with a little loss in yields. Just a personal preference though.
We'll soon find out if I'm a chemist or not!

[goiterjoe]

You're going to have trouble getting clean crystals if you skip steps like that.  I would say skip the epoxide extraction step, as it doesn't seem necessary, but don't skip the ketone distillation step.  If you do, you are going to have some nasty looking toluene extracts after the reductive amination. 

If you really want to skip the ketone distillation, at least distill the MDMA freebase oil after amination.

[pickler]

Skipping ketone distillation is a big no no. Swim skips some steps, but doesn't skip that one. Swim agrees with ya goiterjoe.

We'll soon find out if I'm a chemist or not!

[GuySmiley]

What does tap off mean??
Cause its so fun!

[Rhodium]

Guy: Opening the stopcock at the bottom of a separatory funnel, draining the densest liquid layer into a beaker or whatever. See

Post 305470

(Rhodium: "Acid/Base extraction technique", Methods Discourse) for details.

[SuperStar]

SWIM is only contemplating skipping the DCM step after the Oxone treatment. Still vac distills safrole, iso, ketone
Pardon my friend officer, He's a little slow.