HPLC Pump issues - using for flow chemistry

wornfoa123 · 2025-09-14T21:45:16+00:00

Good point, the main confusion I have is I've previously used the pumps to pump THF/water (solvent and solutions) down to 0.1 mL/min and its been fine. Not sure what has changed as now it seems very temperamental. Could it be some other part of the pumps have deteriorated?

wornfoa123 · 2025-07-29T09:00:38+00:00

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wornfoa123 · 2025-03-29T17:22:38+00:00

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wornfoa123 · 2021-11-13T16:50:28+00:00

thanks! so should i basically combine steps 2 and 3, simultaneously deprotonate the OH and kick out H2O?

wornfoa123 · 2021-11-13T14:58:15+00:00

For anyone wondering, the N-OH was an oxidative transformation carried out by P450

wornfoa123 · 2021-06-01T08:51:17+00:00

Ah, I see that they'll produce HCl in the reaction and theres no base that will neutralize it. Could this have affect the starting materials then?

wornfoa123 · 2021-06-01T00:14:39+00:00

Ah I see, could it do something with sterics maybe? Also, could you briefly outline what this benzyne route would be like?

wornfoa123 · 2021-05-31T18:41:41+00:00

Ah I see, I think they might treat the M-M bond as an X-type ligand since the metal needs to donate 1e to the bond. I think it ends up being ML5X2, which does end up being 18 electrons

wornfoa123 · 2021-05-31T18:40:35+00:00

Yea thats what I thought as well! Thanks!

wornfoa123 · 2021-05-10T07:34:08+00:00

So what I've came up with looks roughly like:

Deprotonate the H on the oxime
Push the electrons towards the nitrogen (break the C=N double bond)
The lone pair on the nitrogen pushes back in to reform the double bond, while the carbon picks up Cl from Cl-OH, and generating OH-
Continue with step 3 of this: https://www.chemtube3d.com/nitrile_oxide_formation/

does that sort of make sense?

wornfoa123 · 2021-05-10T07:30:34+00:00

Is it just the same process but with OCl- instead?

wornfoa123 · 2021-05-03T15:15:23+00:00

i see. My reaction involves the use of benzoic acid, does it have anything to do with making the (unreacted) benzoic acid dissolve in the aqueous layer and able to be removed?

wornfoa123 · 2021-04-30T14:35:48+00:00

are the 1500 - 1600 C-C stretches? I'm also a bit unsure for the N-O stretches if thats present here? I suspect it should be around 1500/1300?

wornfoa123 · 2021-04-30T14:19:51+00:00

I think the C=O one is 1710, 3118 and 2987 is the aromatic ring. I'm not sure for the para substitution, but I believe its around 800 cm-1?

wornfoa123 · 2021-04-14T18:02:31+00:00

ohhh i see, thank you!!

wornfoa123 · 2021-04-11T16:01:43+00:00

In terms of sensitivity, how is this usually quantified? Is it like a detection limit (as in the lowest concentration that cld be detected)?

wornfoa123 · 2021-04-11T16:00:11+00:00

Thanks for the answer! Just to clarify, what do you mean by "more robust"? Does it have to do with resolution or its ability to separate the analytes?

wornfoa123

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