Synthesis of CD3

GLS · Jul 16, 2018

Looks a lot better this time. Personally if I were carrying out the above I would swap out the tin step with an iron reduction, and substitute Dess-Martin periodinane for the PCC; I have never liked the latter as it's too water-sensitive, and the by-products are horrendous.

Rudeofus · Jul 16, 2018

Of all the compounds which might eventually cause problems with acquisition for E6 processing, CD-3 is just about the last one I would worry about. It's still used in abundant amounts by RA-4 process and therefore not at all limited to analog work flow. HQMS-K, also potentially in danger, fortunately can be and has been synthesized with simple lab equipment. I would at some point in time worry about Citrazinic Acid and DTOD becoming unavailable or horribly expensive.

Anon Ymous · Jul 16, 2018

Rudeofus said:
... I would at some point in time worry about Citrazinic Acid and DTOD becoming unavailable or horribly expensive.

Citrazinic acid might not be too difficult to make, there used to be a YouTube video about it. DTOD, while being an ingredient of a "proper" E6 CD is IMHO not absolutely necessary. I've followed stefan4u's formula that uses KSCN and the results were fine. Obviously, I haven't made any side by side testing to compare a "proper" E6 CD with the one using KSCN, but there's a point where you say you're more than pleased with what you got and trying to source DTOD isn't worth the effort...

GLS · Jul 16, 2018

Anon Ymous said:
Citrazinic acid might not be too difficult to make

Seems fairly trivial (if you have access to an autoclave):

https://patentimages.storage.googleapis.com/10/37/d0/6ecab3a75664dc/US2728773.pdf

As for DTOD, it would be fairly simple to synthesise I'm sure, but would require the use of thiols, which smell repugnant and are very unpleasant to work with (even with a fume hood).

Anon Ymous · Jul 16, 2018

GLS said:
Seems fairly trivial (if you have access to an autoclave):

https://patentimages.storage.googleapis.com/10/37/d0/6ecab3a75664dc/US2728773.pdf

Ah, found the video I was talking about, it was removed from YouTube along with everything else user ChemPlayer had uploaded.

Rudeofus · Jul 16, 2018

I got a quote for some oddball organic compound a few years ago. The compound was a bit more complex than Citrazinic Acid and was a standard product offered by that outfit. The price was in a region where not even milligrams per liter would be feasible, as in hundreds of US$ per gram, in quantities of 100 gram.

The phrase "Seems fairly trivial" is quite misleading, since at least some crucial process steps involve insanely toxic stuff (recall de Fender's post about innocent looking Cloroethanol) and therefore have to happen in a fully equipped lab. These labs are anything but cheap to operate.

GLS · Jul 16, 2018

Rudeofus said:
The phrase "Seems fairly trivial" is quite misleading, since at least some crucial process steps involve insanely toxic stuff (recall de Fender's post about innocent looking Cloroethanol) and therefore have to happen in a fully equipped lab. These labs are anything but cheap to operate.

Nothing in the patent procedure I linked to is especially toxic, apart from methanol, and you won't be drinking the stuff so it's not a problem. And yes, I meant "trivial" for a trained chemist in a lab, and in the sense of the simplicity of the synthesis; effectively a one-pot procedure without multiple discrete steps, purifications etc.

halfaman · Jul 17, 2018

Anon Ymous said:
3) Axelcolor from Italy. Their core business seems to be chemicals for minilabs, but they do sell small quantities of chemicals to amateurs. They have an ebay store and you can contact them through ebay. Don't be put off by the €100 shipping charge, it's just wrong. Ask them for a shipping quote instead. Actually, you can also contact them at this email address, where they are more likely to respond quickly: elisa(at)axelcolor.com. They support paypal. I've bought CD4 from them and everything was fine.

I knew the website http://axelcolor.com/, they have vey cheap C-41 chemistry but shipping costs outside Italy were too expensive (105 €).

Rudeofus · Jul 17, 2018

I am certainly not an expert in toxicology, but what I have read about Mesyl Chloride does not sound like I want this thing near me. There are different degrees of "seems fairly trivial", and posting this phrase in a forum that's mostly geared at amateurs (which certainly includes me) can lead to undesirable results.

GLS · Jul 17, 2018

Rudeofus said:
I am certainly not an expert in toxicology, but what I have read about Mesyl Chloride does not sound like I want this thing near me. There are different degrees of "seems fairly trivial", and posting this phrase in a forum that's mostly geared at amateurs (which certainly includes me) can lead to undesirable results.

The patent does not use mesyl chloride. It employs one or more sulfonic acids, which are very different in terms of their chemistry.

Your second point is fair enough. I should have qualified that remark from the off.

Photo Engineer · Jul 17, 2018

Any organic synthesis done by amateurs is dangerous. This cannot be understated.

PE

GLS · Jul 17, 2018

Agreed.

Synthesis of CD3

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