SWIM remembers how irritating it was to not have access to ether for extractions, so here is an easy way of extracting it from a readily available consumer product. Warning - This extraction is hazardous and not for amateurs.

It involves alittle distillation gear, proper safety awareness, laboratory skill, and automotive starting fluid. It must be automotive, starting fluid for your charcoal grill will not work lol. Most brands are 25% diethyl ether, but some can be as high as 50%. Hope this helps fellow mad scientists.

Here is the write-up SWIM created:

Procedure:
Reagent diethyl ether may be prepared as follows. Construct an airtight distillation setup with a vacuum adapter going from a collection flask and hosing connecting from that to outdoors for proper ventilation. DANGER - Ether is extremely flammable and vapors must not be allowed to collect indoors or risk an explosion/fire. To a 1000ml round bottom flask add 500ml automotive lighting fluid (50% ether/50% heptane +CO2). Add a stir bar or boiling chips to prevent bumping. Fit the 1000ml flask to the distillation setup and attach a 250ml flask on the other end, cooled by an ice bath. Be sure to use a decent length condenser and ice cold water for the distillation, a super cooled acetone or IPA + water mix ideally. Begin heating mildly. Ether has a boiling point of only 34.6° C, so condensation will begin quickly. The diethyl ether that comes over should be quite pure enough for most uses. If storing for an extended period of time, the ether should be stabilized with BHT or solid KOH (in order to prevent explosive peroxides from forming) and put in an amber glass bottle. Yield is around 250ml diethyl ether.

hmm, vapor pressure is too high for a water-cooled condenser. it'll work, just very poorly.
this calls for a dewar condenser with dry ice and acetone + dean stark trap.

Graham condenser works nicely, there is some loss but not too much.

If you go to a truck supply place you can get large canisters of this starter fluid that is almost 100% diethyl ether.

A few points about working with this stuff though.

1. The vast majority of clandestine lab explosions involve diethyl ether. All is takes is a spark from someone turning a light on or off, or a faulty switch on a mag stirrer, the furnace turning on, dropping something metal that makes a spark etc.

2. If you open a container of diethyl ether without a fume hood, it is soooo volatile that everyone in your building (if not neighbourhood) will be able to smell it, the vapour will instantly fill a room, especially with summer temperatures. If anyone is hip to what that smell is, good chance it will involve a call to the local police. I know if I caught a whiff of it in my building I would freak!

3. You can minimize the risk by chilling both the container of ether and container you are pouring it into (makes it less prone to evaporation).

4. If you are actually willing to risk explosions and police, you do not have the right to endanger your neighbours/family, this should be done in a space where the only person to die in the explosion will be you. Being careful is not enough, accidents happen, what chemist has not broken a piece of glassware?

5. Know that having a clandestine lab accident in your home will invalidate any home insurance you have.

Thanks sister for a bit of reality here. Lot's of people have lost limbs from diethyl ether if not their houses and lives it really is no joke.

Also Kash I would like to make a quick remark or three about your procedure.



Don't ever fill flasks past the half way mark for distillations. Come on now. Lab ettiquette 101. Even in your picture you show the flask only half full.

Also you made NO mention of explosive peroxides!? Distilling diethyl ether to dryness can lead to huge explosions. It's killed people and cost many fingers in professional environments let alone unseasoned people. Even if it's stabilized a starch iodide test is so important.

Also going to agree with benzyme here, a fair amount of that ether is flying right out the window in that diagram. Graham condenser may provide surface area but its just not cold enough. The loss isn't what bothers me, it's the fact that the loss is going straight out of a window lol.

Also you're article looks straight off of Rhodium I don't understand why you went through the trouble to type it into a .doc . The title might be a bit misleading as well. Considering most people don't have distillation glass-ware or safe heating sources at home so "OTC" for DMT-nexus, is a bit of a stretch.

Thanks for the comments, will take them into consideration and update accordingly for others.

SWIM knows how flasks should usually not be filled to capacity for distillations but ether boils pretty smoothly and it wasnt an issue. Maybe SWIM will try a super cooled IPA/H2O solution for cooling in the future to increase yield. Will mention peroxides in the equation, forgot to becuase it seems like it should be common knowledge for anyone attempting such an extraction and thats what the necessity to stablize with BHT is about. The article was not off rhodium at all, created it myself with a modified distillation depiction using the same type template becuase I like the style, so its really not misleading.

People attempting this definitly need to have the appropriate knowledge and lab skills before attempting, and with those in hand this is an easy tek. There is no excuse for ignorance. I think I mentioned explosions and fire no?

Results: An IPA/ice-cooled Graham works quite well. 2x320ml 50% ether + 4x320ml 25% ether volumes were distilled, and then distilled again and stabilized with a pinch of BHT. Theoretical yield 640ml, actual yield was about 575ml ether. Mua. ha. ha.

bold it or highlight it, diethyl ether is no joke.

better yet, use THF instead of ethyl ether, if attainable. it's a cyclic ether that's not quite as flammable (3 rating instead of 4).

Anyone with proper lab skill and knowledge wouldn't need this 'tek'.

Also fire hazard doesn't really cover explosive peroxides. For example, naptha is a fire hazard but you can distill naptha to dryness without any real issues. Although that is still not really recommended under some circumstances. BHT doesn't last forever, starch iodide tests should be performed prior to usage. Also, BHT then becomes a contaminant for extraction purposes depending on concentration, generally low but still.

The problem with THF is that it is miscable with water, although it can also be found OTC and distilled. Diphenyl ether can be a reasonable substitute for Et2O in a lot of cases with less of a safety hazard. Although it isn't readily available in a lot of circumstances.

Over-all ethylacetate is a great substitute. Is cheaper, easier to acquire in good purity, safer to handle and work with outside of a fume-hood, etc.

ethers in general will be somewhat miscible with water, because they have an H-bond acceptor. ethyl acetate has two acceptors, thus is more polar, and even more miscible with water.
great extraction solvent, nonetheless, especially for most of the alkaloids of interest.