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TOPIC: Mesochem Daclatasvir NMR results - pls interpret

Mesochem Daclatasvir NMR results - pls interpret 2 years 8 months ago #602

  • ahmad
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Please see the attached NMR results for Mesochem Daclatasvir, which I have got done from my local university's chemistry lab. There were two tests done, one is against Hydrogen and other one against Carbon. As per the NMR technician it confirms the molecular structure of Daclastsvir but there is some minor impurity but he failed to quantify it as he was not expert on the subject. I am posting the results here to seek more expert comments.

NMR Analyser used was Brukker 300 MHZ (don't know if there are any further classification)




Last Edit: 2 years 8 months ago by ahmad.
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Mesochem Daclatasvir NMR results - pls interpret 2 years 8 months ago #605

  • DrJames
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Hello Ahmad,

This is not a very clean spectrum but probably has more to do with the technical execution of the test than the API.

You can find spectral data for Daclatasvir here:

orgspectroscopyint.blogspot.com.au/2015/07/daclatasvir.html

1H NMR (400 MHz, DMSO-έfc, 80 0C): 8.02 (d, J=8.34 Hz, 4 H), 7.97 (s, 2 H), 7.86 (d, J=8.34 Hz, 4 H), 6.75 (s, 2 H), 5.27 (t, J=6.44 Hz, 2 H), 4.17 (t, J=6.95 Hz, 2 H), 3.97 - 4.11 (m, 2 H), 3.74 - 3.90 (m, 2 H), 3.57 (s, 6 H), 2.32 - 2.46 (m, 2 H), 2.09 - 2.31 (m, 6 H), 1.91 - 2.07 (m, 2 H), 0.88 (d, J=6.57 Hz, 6 H), 0.79 (d, J=6.32 Hz, 6 H);

Putting that in an simplified format (first number is ppm on x axis, second is expected y axis value)

8.02 (4 H),
7.97 (2 H),
7.86 (4 H),
6.75 (2 H),
5.27 (2 H),
4.17 (2 H),
3.97 - 4.11 (2 H),
3.74 - 3.90 (2 H),
3.57 (6 H),
2.32 - 2.46 (2 H),
2.09 - 2.31 (6 H),
1.91 - 2.07 (2 H),
0.88 (6 H),
0.79 (6 H);

So if you look at your spectrum you see 12.66 @ around 0.85 ppm - this represents 2 peaks (0.79 & 0.88) merged into one due to instrument power limitations. You can continue on for other peaks, but your spectrum is not great one for teaching NMR basics.

I have attached a pdf showing the impact of concentration on the Daclatasvir spectrum. This was a dilution of exactly the same sample so the only thing different was more solvent. Notice that despite the fact it remained the same API there have been changes to the spectrum.
Attachments:
YMMV
Last Edit: 2 years 8 months ago by DrJames.
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