[Ingeniosuccinimide]

Hello, I have a somewhat weird question, and would appreciate an opinion on my issue. Preferably from a PhD/postdoc or someone who has completed these.

I'm having serious problems with the procedure for one synthesis (which was published in one quite good German paper in the '80s. I was trying to do everything I can to make it work, but without any success.

My supervisor is currently not in his office for a next couple of weeks, and I'm so pissed off that I'm considering writing (of course a polite) mail to the authors of that procedure and ask them what the hell were they doing?!

Is it usually accepted in academic circles that a PhD/postdoc contacts the author of some paper in regard to an issue like that? I asked two postdocs from my department for an opinion, and they were also puzzled...

[Dan]

Yes, it happens from time to time and is perfectly acceptable to do. Nevertheless, you should seek advice regarding the procedure from more experienced colleagues (and definitely from your supervisor) before attempting to contact the authors.

If the paper was published in the 80s, I very much doubt you'll get anywhere. While the PI might still be active and easy enough to track down, bear in mind that the experiment may have been done by a student in the lab. In any case, whoever did the experiment is unlikely to remember it in sufficient detail after 30 years to be of any more help than someone closer at hand.

If it was me, I wouldn't contact them.

You could explain what the reaction is and what you have tried here on the forums (and give a citation) and we can try to help you - that will probably be a far more productive use of your time.

[Babcock_Hall]

I would contact them, but I would also do what Dan suggested.  I have occasionally had success in doing so, even in one paper that was older than the one in question.  However, it is important to keep the tone of your message polite.  I would be tempted to use phraseology along the lines of, "this procedure has not worked in our hands," as opposed to something more confrontational.

[Ingeniosuccinimide]

Thanks for replying. If you have a minute or two, I would love to hear your opinion on this really weird procedure. It is quite brief and it can be found here:

http://www.sciencedirect.com/science/article/pii/S0040403900842938

I'm trying to make benzenesulfinyl chloride. It is done by dissolving PhSSPh in acetic acid (I presume pure, since the product is very unstable in presence of moisture) and adding sulfuryl chloride dropwise. However, the procedure states that the mixture of PhSSPh and AcOH should be cooled down to -40 degrees and well stirred before adding SO2Cl2, and my mixture freezes around -10 degrees!! The two postdocs I asked were also puzzled by this, because we simply don't understand what the hell did the Authors do. 

[curiouscat]

Have you tried doing it at whatever Temp. you find it just freezes at?

How much PhSSPh are you adding to AcOH? MP depression of AcOH will be very sensitive to that I presume?

[Corribus]

I recently contacted an author of a paper from 1993 about some data in a figure, and he was able to send it to me.  This is why there is always a corresponding author.  Occasionally it can be difficult to track these people down, particularly if they've switched organizations since the paper was published.  However you can usually google them to find out where they are now.  Worth a try, certainly.  In my experience, people are usually thrilled that someone was interested enough in their work to contact them.

[Ingeniosuccinimide]

Have you tried doing it at whatever Temp. you find it just freezes at?

How much PhSSPh are you adding to AcOH? MP depression of AcOH will be very sensitive to that I presume?

I use the exact amounts described in the procedure. Tried doing it for a couple of times, the mixture freezes around -15° C and if I do the reaction under that condition, the unwanted side-products form. Somehow I should get down to -40° C, I tried with acetic anhydride but it didn't work. I was considering some inert solvent, but for this type of reaction I really don't know what could be used (and unfortunately don't have enough time to test a dozen of solvents...). I would really appreciate an opinion on that.

 I actually wonder what the hell did the authors do in the original paper...