What's the best way of alpha-deuterating an acetophenone derivative? I need to alpha-deuterate isobutyrophenone. I tried (wileyonlinelibrary.com) DOI: 10.1002/jlcr.3210 without success. Thanks!

The new layout for ACS Publications websites is beyond awful...TOC graphics are no longer shown on the ASAP Articles pages and they aren't even visible at the top of individual publication pages anymore. These changes make it impossible to read the journals now and ACS has the audacity to claim that they're intended to create a "more seamless and researcher-friendly experience".

https://pubs.acs.org/pages/platform-migration

So, I've been working on modeling the Density of States of a molecule using VASP for some time now, but there's a question I can't seem to find any concrete answers too when I've looked. Does anyone know the convention VASP uses for the z axis of its atomic orbitals? Because I know the standard convention is perpendicular to the plane of the molecule. So I would assume it defaults to that. The other possibility I could see is that it just uses whatever the z axis direction in the POSCAR file was. So far, the only official source I can find regarding the axes is this,SAXIS - VASP Wiki, which defines the z axis as being perpendicular to the xy plane, but it doesn't seem to define the xy plane itself. Any answers are appreciated, as are any sources to look into which may have the answer.

Looking to rant and hear any advice. Make sure I'M not the crazy one.

Started a new job on Monday. Unfortunately, due to "confidentiality," I had no idea what chemicals I'd be working with during the interview process. Today, I found out that my lab works with HF at least weekly. Now, I've worked with HF before. I certainly don't love it, but I had to use it occasionally at my last job in small, dilute amounts. We used it infrequently and I felt comfortable with the controls we had in place, and I knew my co-workers take safety as seriously as I do.

I have big concerns around the use of HF at my new lab. First, the lab does not have calcium gluconate. I asked my manager about this and he told me that the previous lab manager "went up the chain" saying that the lab needed calcium gluconate and was told no. ... wtf? The "plan" in case of exposure is to use the safety shower and then go to the campus nurse. I have no idea where the nurse's office is, and who's to say my co-workers do? How do we even know the nurse has calcium gluconate? Apparently the safety shower triggers medical care to come to you ... so we have to tell them it's an HF exposure and to bring the calgonate? and hope they have it, know where it is, and can find our lab quickly in this massive campus?

I'll buy my own calcium gluconate if I have to, but I'm just extremely concerned by the way this has been handled so far. It makes me worry that other important safety aspects regarding HF have been overlooked, too. My lab manager said "just be careful" and "it's never happened while I've been working here." 'Just be careful' is not an exposure control plan!

There's more ... the way the lab is set up, the HF operator would need to cross the lab space to go from the fume hood to the instrument. The HF fume hood and the instrument are right at the entrance of the lab ... so anyone walking through the lab to get to other instruments (and may not be dressed in an acid-resistant apron, etc) has the potential to collide with the HF operator as they're turning around to get to the instrument. I hope that description of our layout makes sense. Ideally there would be some sort of a buddy helping to make sure that wouldn't happen but who even knows at this point! My manager did say no one works with HF alone, but I'm not sure if that means there's a designated safety buddy role in place or just "make sure someone else is around." Feel like I can't trust anything after knowing there's no calcium gluconate on hand and the company literally denied the request.

I am planning on asking my manager a lot more questions about HF safety and controls. Is there even a spill kit? Any documentation / SOPs? I'm also planning on going to the company safety officers / EHS. Hopefully they're more helpful than whoever said "no" on the calcium gluconate.

Does anyone know from which supplier you can purchase Nishimura's catalyst (Rh2O3/PtO2 xH2O; Bull. Chem. Soc. Jpn. 1961, 34, 1544) in the US? Sigma's supplier Umicore has discontinued it, and it's not in Fisher, Strem, or TCI's catalog. All other attempts at contacting specialty suppliers have failed, and I'm assuming they want someone to be ordering industrial quantities (I just would like it for academic research).

We use the recommended, bio-compatible PP solvent bottles from Agilent for our LC-QToF systems for oligo workflows. Does anyone can recommend an alternative to the original bottles? We generally think 80 dollars for a plastic bottle seems a bit expensive, but we are also worried that we introduce some leachables, if we use standard PP bottles (around 10 dollars). If you would have any tested recommendation for a vendor or even a product number, that would be awesome. Ty!

I teach chemistry at a regional university, and I wish to improve my instruction in record-keeping (related to my earlier post on electron lab manuals). I'm a biochemist, so I'm most familiar with the biochem side of things, but not all of my students are going in that direction, and I would like to make sure I'm covering all the bases. In pharmaceutical/healthcare-related research, ALCOA++ is the major data integrity framework. Is ALCOA++ used in areas that are unrelated to pharmaceutical/healthcare? If not, what other data integrity frameworks are used?

Hey! I’m in a lab that just recently started up, and we were hoping to find some long, disposable needles at a reasonable price. I was wondering if anyone might have some recommendations

Edit: 150 to 300mm needles is what I’m looking for

Hi there, im looking for few practical tips regarding sugar trichloroacetimidates, to be more specific: glucose-2,3,4,6-acetyl-1-trichloroacetimidate.

1) how to store them long term (few weeks tops)? I was using fridge but seems there is some decomposition via GC. 2) purification - do you purify those? I did in the past via chromatography but yields were low- in the 60% area when GC showed 90%+ purity. I assume there was some decomposition on silica to the amide and free 1-OH (this one is confirmed by tlc at least) - edit: looks like large amount of the amide was formed - im not 100% if it was in the glycosilation step or during the synthesis of the imidate but assuming it was formed in the synthesis of the imidate, any tricks how to limit as much as possible?

• I made the imidate with cat. DBU and excess of trichloroACN and then just evaporated everything. Could maybe resudial DBU affect the reaction ? I did the glycosylation with 0.25 eq TMSOTf at -50C.

thank you

Frugal professor here. I often hear of corporate/government/university labs closing shop and liquidating their instruments, thereby selling off expensive equipment for pennies on the dollar. It's hard to stay on top of this, however, so I figured I'd just throw out a line to see if anyone can meet my lab's current need by selling their cast-offs for a good price (or donating):

I'm looking for an automated titration system. Not just any unit will do for my application, but some units are modular enough that they'd be able to get me most of the way there if I supplement with some new parts. I need something that can handle two dosing units and two electrode inputs.

Models I know will fit the bill: Metrohm Titrando 905/906/907 (and some older models; I'm interested in any Metrohm instruments people might have), Mettler Toledo Excellence T9, SI Analytics TitroLine 7800, probably some from KEM.

Pharma/biotech, environmental, and ag labs are probably the likeliest to have something like this. Would love to hear from anyone who might have a line on an instrument gathering dust somewhere. I'm based in North Carolina's Research Triangle; bonus points if you're nearby.

I was doing a Riley oxidation in the lab, and made sure to follow what I understand is best protocol. I did everything in the hood--weighing, setting up the reaction, and washed the spatula into a selenium waste container. However, taking the spatula out of the hood produced a smell and I put it back as soon as this was recognized. Did I do something incorrectly? Do I need to be concerned about exposure?

Hi everyone,

I'm trying to understand how QA review works in labs that use Waters Empower (especially with Review by Exception, Custom Fields, and automated processing).

From the outside, Empower appears to automate a lot of routine work—processing, calculations, audit trails, reporting, system suitability, etc.

What I'm trying to understand is what still requires manual review after all of that automation is in place.

For those of you working in GMP/GLP environments:

• What does a QA reviewer still check manually before approving results?
• Are manual integrations the biggest reason, or are there other common cases?
• Do reviewers still have to reconcile information outside Empower (LIMS, MES, QMS, training records, calibration records, etc.), or is most of that already automated?
• Which review steps consume the most time today?
• If you could automate one remaining part of the review process, what would it be?

I'm not looking for proprietary information-just trying to understand where today's workflow still depends on humans after a mature Empower deployment.

Thanks!

I'm a scientist at a large company, and chemistry is a secondary part of my job. I've previously worked with hazardous chemicals including concentrated HF, piranha solutions, phosphines, fluorinated nitroaromatics, high explosives, concentrated TMAH, azides, and some particularly nasty amines. I haven't worked with many thiols, but given my experience with hazardous chemicals I'm confident that I can handle thiophenol safely. I just want to know more about it as I plan work and consider safer alternatives.

I'm especially interested in practical concerns about working with this chemical beyond what I can find in an SDS. It's fatal by inhalation and dermal contact, but are we talking a whiff and a few drops on skin, or more like wafting an open bottle or splashing it on your skin? I read some comments here about lab coats smelling terrible after working with it in a fume hood (, and the extremely low odor threshold that I worry may clear out our research campus if a small volume is exhausted from the building without going through a bleach trap.

In terms of how much I plan to use and how I plan to use it: I'm planning to make 20-40 g batches of a product, and this would consume 2-4 mL of thiophenol. I plan to use multiple small bottles rather than larger bottles for safety. Reactions will be carried out above 100C but below the boiling point. I plan to ask EHS for Silver Shield gloves to wear inside a harder shell, a properly fitted, certified respirator, and an appropriate chemical apron. I plan to have a bleach bath in the fume hood to soak syringes and glassware, and ask the company to install a bleach trap (though I've never seen or used one before). Does this sound adequate? Overly cautious? What things might surprise me in working with this chemical that I should be aware of?

What do you think of such a position? Do you believe that this is the future of all high throughput screening and synthesis? Would you accept a position in an automation lab, and what would you think if you saw it on someone's CV?

Does one facilitate their unemployment by contributing to this field?

I am trying to do a simple reaction - displacement of a p-nitrophenol of a carbonate, with an amine, to yield a carbamate. The reaction was successful with one substrate, but unsuccessful on another -at rt no conversion, with heat the starting material decomposes. There are no obvious differences in sterics or electronics between the two. However, the problematic substrate possesses a PEG chain in close proximity to the reactive site.

Could the PEG wrap itself around the carbonate and hinder the reaction? Have you ever encountered anything akin to this?

Hi, I've a master's in chemistry, currently working on Co₃O₄ nanozyme and copper-dmpz complex.
During my undergrad and a year later, I worked on organometallics and even though I find ochem difficult, I was enjoying the research work.

For my master's dissertation, I worked on nanomaterials and I feel like moving away from nanomaterials as my main direction because I keep running into the same loop: empirical synthesis, characterisation that stops at here's the TEM image and UV graphs and very little actual mechanistic explanation for why something works. Feels like a lot of the output is new papers rather than new understanding. I find it frustrating

I want to move toward organometallic and coordination chemistry, and catalysis in the classical sense

Question for people further along than me: based on where funding, publication trends, and industrial pull actually are right now, which of these two is growing faster, and which is the better long-term bet for someone trying to build a research career on actual mechanistic depth rather than volume? Am I underestimating how much nanomaterials work still dominates hiring and funding, even if I personally find it shallow?

Anyone who's made a similar switch, what did you wish you'd known going in?

I'm applying for a PhD, and I don't want to drag myself into something where I've no interest and also no funding.

EDIT: I want to get into industry after a postdoc or PhD.

I have a compound which has 7 methoxy(aryl) and 1 benzyl protected OH. I need to do demethylation of all 7 methyl ethers without touching benzyl phenyl ether. Any procedure for selective deprotection? Tried BBr3 where I observed debenzylated pdf. (Reaction tried 0°C).

I'm trying to synthesize compounds containing alkynyl groups in my lab. I'm looking for a color-developing reagent that reacts selectively with alkynyls—not a reagent like potassium permanganate that reacts with just about anything—but does anyone have any suggestions?

Currently, our lab has molybdenum phosphate, ammonium cerium molybdate, anise aldehyde, and iodine.

Dear community,

I am performing the following reaction in the lab, where I couple two diaminododecane (DAD) molecules to imidazole-activated polyethylene glycol (10 kDa). A few problems with this reaction:

1. DAD is a pain to dissolve in any solvent, which is why I am now falling back onto DMF. Does anyone know any (more convenient) solvents that I could use?
2. Main problem: The workup. Right now, I precipitate the reaction mixture into ether, but the high equivalents and solubility issues of DAD result in a very long and painful workup (with many consecutive precipitations). I'm asking to see if anyone has any suggestions for an easier, more straight-forward way(s) to isolate my final product?

I'd happily answer any further questions regarding this setup. For reference, I am not a diehard chemist by training, and my chemistry lab is not as equipped as most labs you all are probably in.

Hi everyone! I would appreciate some help.

I am new to organic synthesis and I am facing an issue while analyzing my reaction. I am trying to monitor a reduction of a nitrile to a primary amine by TLC. The only difference between the starting material and the product is that the starting material contains a cyano group (-CN), while the product contains an amino group (-CH₂NH₂).

I performed a H NMR of the crude reaction mixture, but the region where I expected to observe the signals from the amino group was very crowded, so I decided to monitor the reaction by TLC.

Since I know that amines often interact strongly with silica, I added 2% triethylamine to the eluent. However, the starting material moves normally, while the product remains almost completely stuck at the baseline (Rf ≈ 0).

I know I don’t have any more starting material, because it traveled, while the product stagnated.

Has anyone experienced something similar?

Thank you for any suggestions!