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Topic: Starting Material and Product have same mass  (Read 2495 times)

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Offline phenol2015

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Starting Material and Product have same mass
« on: March 12, 2015, 04:04:27 AM »
Hi,

I have a reaction where my starting material and product have the same mass. I'm reacting an amine with a tyrosine (O-bounded amino acid) ester. If the reaction succeeds, the amino acid O-bounded to the tyrosine should transfer onto the amine to form an amide with a free amine, and the tyrosine would form the free tyrosine phenol.

Are there any analytical techniques that anyone out there can recommend me using? I make very small quantities at a time and have tried to find a way of proving it but everytime, I can't seem to prove it because my data doesn't show anything.

Many thanks in advance.

Offline kriggy

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Re: Starting Material and Product have same mass
« Reply #1 on: March 12, 2015, 07:35:43 AM »
Use HPLC-MS, your products are going to have different retention time. If you analyze your statring materials, then from their retention times you can clearly see what peak belongs to your products and what to your unreacted starting material

Offline phenol2015

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Re: Starting Material and Product have same mass
« Reply #2 on: March 15, 2015, 06:38:14 PM »
Thanks. How should I monitor my reaction then? I don't know how long the reaction takes.

Offline discodermolide

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Re: Starting Material and Product have same mass
« Reply #3 on: March 15, 2015, 08:57:33 PM »
As Kriggy said you can use HPLC for reaction monitoring, just leave out the MS part and use UV detection.
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Offline kriggy

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Re: Starting Material and Product have same mass
« Reply #4 on: March 16, 2015, 10:44:53 AM »
Thanks. How should I monitor my reaction then? I don't know how long the reaction takes.

Then take samples in time intervals. I like to take one after the reaction is going on for onehour and then from comparing areas of your starting material and product in you can get some idea how fast the reaction is going

Offline phenol2015

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Re: Starting Material and Product have same mass
« Reply #5 on: March 30, 2015, 08:45:48 AM »
And in terms of separation, what's the best approach to isolating my product?

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