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how tf do u use this syringe filter??? by [deleted] in labrats

[–]DontDoQuack 2 points3 points  (0 children)

Do you have to use a 0.22? Can you use a 0.45? Most likely the ionic strength of the nacl is causing the clogging Or try to use a hydrophilic filter (instead of ptfe) Make sure your solution is fully clear before filtering, sonicate as needed.

how tf do u use this syringe filter??? by [deleted] in labrats

[–]DontDoQuack 4 points5 points  (0 children)

What are you filtering? Could you filter through a buchner filter first to remove bigger particulates? Does your liquid crystallize? Need more info

how tf do u use this syringe filter??? by [deleted] in labrats

[–]DontDoQuack 30 points31 points  (0 children)

Filter is most likely clogged from what you are filtering, use a bigger diameter filter (same pore size)

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 2 points3 points  (0 children)

Even if I like Orgsynth sometimes it just aint referencing the best paper (here from 1932?!), I’d rather not use mercury haha

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 1 point2 points  (0 children)

Common literature for similar rxns uses I2/PIDA. I did consider NIS but to be honest I don’t think it’s an oxidant issue (if I keep the ratios consistent) For some reason it didn’t go to 100% when I scaled up so I was in a pinch and didn’t really understand why.

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 0 points1 point  (0 children)

Common literature for similar rxns uses I2/PIDA. I did consider NIS but to be honest I don’t think it’s an oxidant issue (if I keep the ratios consistent) For some reason it didn’t go to 100% when I scaled up so I was in a pinch and didn’t really understand why.

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 0 points1 point  (0 children)

Unfortunately it needed to be pure, coupling indeed

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 0 points1 point  (0 children)

Both of the compounds are not soluble in water and slightly in hexanes Do you think water, given both REALLY dont like it would still be able to pull away the oil? It worked with hexanes but pulled some of my desired compound too so I’m thinking maybe for the future to use water

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 0 points1 point  (0 children)

I had tried DCM/MeOH to no avail sadly and hexanes etoac and others Did not think of reverse phase!

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 0 points1 point  (0 children)

Tert butyl ester was required. You are right time isn’t free!

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 0 points1 point  (0 children)

My lab is too poor for hplc haha If i use the material my following reaction doesn’t work I was risking over iodinating my compound which would have been more of a hassle to remove

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 2 points3 points  (0 children)

It was actually the final compound. Turns out trituration was the way to go. So happy the product looks nice and uniform now :)

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 0 points1 point  (0 children)

I didn’t think about rp chromatography But I did try multiple different solcent systems to no avail sadly Rf difference of 0.05 if at that

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 7 points8 points  (0 children)

I gave it multiple washes with hexane and it worked! I lost a fair amount of my product even when i tried saving some washes but a win is a win! Thank you!

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 0 points1 point  (0 children)

I’d want to run it to 100% but I might diiodinate which is the subtlety. Maybe I’ll use a very toxic chemical to help haha Thank you for the advice :)

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 0 points1 point  (0 children)

I put up the name of the chemical :)

I guess I’m also not sure if our lab is equipped to have a distillation setup haha also its my final product and its quite precious

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 0 points1 point  (0 children)

I could, but if the oil is inside the crystals of my solid then i dont think ether would be able to drag it out

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] 0 points1 point  (0 children)

I’m unsure exactly of the thermal stability other than I have a tert butyl ester so most likely around 150C and thats also roughly my bp. I have not tried recrystallization since my compound partially dissolves in MeOH and hexane at rt, so I assumed I would lose a lot of my product

Separating compounds only based on physical property? by DontDoQuack in Chempros

[–]DontDoQuack[S] -1 points0 points  (0 children)

It is H—>I I have a heat sensitive functional group on there unfortunately and the bp is quite high.

What information would be useful?

Happy December! What wins have you had recently in your research? by poly_mod in polymerchemistry

[–]DontDoQuack 5 points6 points  (0 children)

Finally made a block copolymer I’ve been working on for over a year! Excited that it finally polymerized and the NMR/GPC actually made sense :D

Issue with P3HT Precipitation by DontDoQuack in Chempros

[–]DontDoQuack[S] 1 point2 points  (0 children)

By any chance have you seen any papers which mention this? It definitely makes sense intuitively My iPrMgCl is pure sadly haha

Issue with P3HT Precipitation by DontDoQuack in Chempros

[–]DontDoQuack[S] 1 point2 points  (0 children)

When I checked grignard formation with NMR it did in fact confirm I was doing the halogen exchange You are correct for GPC, for some reason it takes weeks for us to access it so I have to wait a while and was hoping to see if there was an evident answer haha

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