[rolnor]

If I get a commercially avalable compound as final product in a experiment, is it enough to wright "spectra are consistent with those of a commercial sample" in the experimental and include a proton NMR in the supp. info? This is for JOC.

[chenbeier]

I would put in the NMR taken by yourself and maybe a comparison of the commercial product.

[wildfyr]

Everyone will hate you for not including spectra in the supplemental. If they are using your procedure or looking to compare their NMR of said compound to a lit one, its really annoying when they find your paper doesn't have it. Think of all the times you've been hunting for some reaction from 1972 and all the paper says is "Prepared according to method by Romero et al in the French Journal of Definitely Never Translated To English 1948 at 89% yield." I literally curse aloud when that happens. This is the same thing.

Finally... its not like Pfizer publishes their NMRs in the little booklet with the drug, most people would end up looking in academic lit for such a thing.

JOC Usually wants NMR and Hi-res mass spec for compound identification anyways.

/rant

[rolnor]

I think you missread wildfyr, I will include a proton NMR in the suppl. The compounds are very simple, like 3-(bensyloxy)phenol and my spectra are very clear. I dont think you need HRMS for known compounds for JOC?

[wildfyr]

OH! I apologize. I think that is perfectly fine. Only need HRMS for a new compound or if there is any doubt of identification.

Sorry for the rant then, it was undeserved.

[rolnor]

I gave you a "snack"  wildfyr, that seems very good! I have studied the guidelines for authors very carefully but some things are not completely clear.

[phth]

I gave you a "snack"  wildfyr, that seems very good! I have studied the guidelines for authors very carefully but some things are not completely clear.

1 line of evidence is enough. You can be asked to provide the proton, so it's best to just include it. You can report Rf data too, for example.

[blackcat]

4 years ago when I submitted my paper as corresponding author to JOC, I found the requirements for synthesis for this journal is obviously more rigorous than other journals I have considered.

Sorry I forgot the details, but I remember there should be a checklist for the compounds (especially the final one).

Back to your question, it certainly helps if your spectra matches with commercial or authentic sample. However, NMR spectra may not be convincing enough to tell about purity. If you are dealing with other journals like Dyes and Pigments and JMCC, you will likely pass. For JOC, I am not entirely confident.

[phth]

4 years ago when I submitted my paper as corresponding author to JOC, I found the requirements for synthesis for this journal is obviously more rigorous than other journals I have considered.

Sorry I forgot the details, but I remember there should be a checklist for the compounds (especially the final one).

Back to your question, it certainly helps if your spectra matches with commercial or authentic sample. However, NMR spectra may not be convincing enough to tell about purity. If you are dealing with other journals like Dyes and Pigments and JMCC, you will likely pass. For JOC, I am not entirely confident.

Your data can be called into question. Reported reagents, HRMS datafiles, etc. The corresponding author is required to provide the data if a structure is misreported, for example. There are many instances where NMR spectra are assigned incorrectly. The paper can be retracted/corrected depending on the severity.

[rolnor]

I am not sure what you mean, if I have very, very clear 1-H and 13-C NMR on my known compounds and they are easy to assign I can not really se any problem? They state very clear that for known compounds the author should not include detailed NMR data, only include a proton-NMR in the supplemental info?

[blackcat]

I am not sure what you mean, if I have very, very clear 1-H and 13-C NMR on my known compounds and they are easy to assign I can not really se any problem? They state very clear that for known compounds the author should not include detailed NMR data, only include a proton-NMR in the supplemental info?

I know you may have super NMR, however, NMR has sensitivity issue in terms of purity determination. Normally people prove purity by elemental analysis and/or HPLC. Because you are now dealing with JOC, the journal is more demanding in the synthesis part and hence NMR spectra alone for final compound may not be enough.

[rolnor]

I think you need to read Guidelines for Authors on acs homepage, the rules for purity is really not so demanding. I feel I repeat myself, a well-resolved proton-NMR is fully satisfying for known compounds. For new compounds you need HRMS or elemental analysis and also carbon-NMR.

[hypervalent_iodine]

IME, the only o chem related journals that care about purity analyses are med chem ones, particularly J Med Chem, which requires that any compounds you use for testing have HPLC or EA performed, which is then given in the SI.