Methyl Man's MeOH version of the benzoquinone wack

[NedKelly]

Just a few little questions for the bee's in the know about the about dream
1.......would you recommend this for a first timer ?
2 ......will it scale up OK , like around 6 Lts of sasafass a go ? , hopefully once I master it
I figure if your going to do it you should make it worth your while
3 ....Is there a cheaper alternative than Paladium 2 Cloride ?
4.......can I recycle the catalyst like I do with my RP ?

[Vitus_Verdegast]

1: Yes
2: No. Do multiple smaller scales, less room for error for a first timer . And please use pure safrole and not straightup sassafras oil!!
3: Nope
4: Nope. No succes in separating palladium from all the precipitated hydroquinone that I know of.

These questions could also have been easily answered using TFSE (and using correct English spelling of course).

[nitrous351]

I agree with Vitus as long as you can safely (i.e., without getting arrested or put on a watch list) acquire the benzo and the PdCl2. It's a very easy reaction to do, but be extra cautious when working with the benzo... it's nasty stuff (wear lab coat, goggles, and gloves...respirator recommended, good ventilation NECESSARY)<---- downsides to reaction
If you're not sure you can get the reagents safely, or you can't properly provide yourself with adequate safety for this reaction, I would recommend going with the peracid or oxone reaction.
These reactions are also very easy to do, and the reagents used are MUCH less suspect and are safer. good luck peace

[Rhodium]

can I recycle the catalyst like I do with my RP ?

Take a look at

Post 415909 (missing)

(Rhodium: "Red Phosphorous isn't a catalyst!", Stimulants) where I explain the following:

Red Phosphorous is not a catalyst, it is the actual reducing agent in the RP/I₂ reduction of (pseudo)ephedrine, any red powder which you are able to filter off after the reaction is either 1) excess RP which wasn't consumed in the reaction, or 2) if you used RP from matchboxes, it may also consist of glass powder and phosphorous pentasulfide (P₂S₅) which also are included as additives in matchbox strikers.

In the case of PdCl₂, the catalyst isn't spent after the reaction, but it may be present as a mixture of both palladium(II) salts, as well as elemental palladium powder, making it hard to isolate it using a specific procedure from the considerable amount of other gunk present in the post-reaction mixture, besides the product MDP2P. The palladium is still there, it's just that noone has been able to devise a working method for recycling it and converting it back to the desired PdCl₂ form again (but you can find a lot of posts on the topic by searching on "palladium recovery" in TFSE).

[NedKelly]

Which method would you guys personally recommend for larger scale dreams of about 5 to 6 ltrs of safrol , once I'm up to it .

[nitrous351]

on several factors. PdCl2 is quite expensive, and you would need a lot to run a multi-liter reaction. Also, benzo is a hazard, and you should take that into account. The benzo wacker is not very environment friendly, especially if you don't have access to proper waste facilities. The upside is that it's an easy reflux, and the yields are good.
The peracid or oxone methods are equally easy (if not easier) than a benzo wacker. The yields are a bit lower than a benzo wacker, though. The upside to these reactions are easiness in procedure and easiness in obtaining reagents. good luck peace

[technology]

Dude,

I think you are trying to run before you can walk.. i admire the aspiration, but slow down, one step at a time.

first, pull of your first synth then question a scale up, i am not harrasing you, just stating an opinion that you either acknowledge or reject..

either way all the best

TECk

[NedKelly]

[runne]

I agree on studying the procedures that are going to lead you wehere you want to go, but I also think there are ample examples in the search engine about the scale up of most of the common procedures - including benzo stuff.

As an example, oxone can scale up huge - as long as you use 55gallon barrels! I think the caution that technology is saying is more along the lines of turning your 5 liters or whatever of good stuff and turning it into unrecoverable crap. Shit happens - in the lab as well.

[technology]

Always, buy more than what you need anyhow, that is a number one rule when it comes to chem purchase.

Yes, buy lots and lots, but start small, then work on up, gradual or double, it is up to you.. i am merely pointiing some advice, and just like all, they either refute it or support it, the choice is yours..

all the best