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1answer
59 views

How do I remove tetrabutylammonium perchlorate from an organic synthesis?

I am trying to remove tetrabutylammonium perchlorate (TBAP) from an organic synthesis where TBAP was used as an electrolyte. I am working with compounds containing the amide group. I have used flash ...
0
votes
1answer
114 views

How to remove MEHQ from Methacrylic acid monomer without reduced pressure distillation?

I am aware that the standard way to remove MEHQ from Methacrylic Acid is to perform reduced pressure distillation. The papers I see suggest using ~ 10 Torr pressure to perform distillation. Sandler's ...
1
vote
1answer
2k views

Synthesis of Benzaldehyde and Aniline Schiff Bases

I have a problem while synthesize the schiff base. I synthesized using absolute ethanol as solvent and use reflux method for 4 hours generally. The problem occur on TLC where there is still two spot ...
2
votes
1answer
152 views

Ester as a side product in the synthesis of bromoalkane from alcohol. Is it correct?

About 5 months ago, I answered a very interesting question albeit a very simple one. Why do we need sulfuric acid in creating alkyl bromide and not in creating alkyl iodide from alcohol and ...
4
votes
1answer
682 views

How to remove pyridine from Reaction mixture containing chiral molecule with diacetal protection group?

While working with chiral molecule, we have pyridine in our reaction mixture. Molecule has four chiral centre and protection group-diacetal and acetyl groups which may break in harsh conditions. ...
2
votes
2answers
622 views

Removing aluminum oxide from impure silica

We have an assay for a mine. Our goal is to have only silica. Is there a cost effective way to extract the contaminants? The product is a fine powder called diatomaceous earth, or fossil shell flour. ...
2
votes
1answer
6k views

Why is the solid product washed with ice-cold solvent during in the last stages of recrystallisation?

Why is the solid product washed with ice-cold solvent during in the last stages of recrystallisation? Is this to remove soluble impurities? (for example) Well, what if the impurities were also ...
2
votes
1answer
1k views

Confirming the presence of 4-bromoacetanilide during bromination of acetanilide

In my lab, acetanilide was added to bromine in aqueous acetic acid, and discolouration of the reaction mixture was obtained, indicating that bromine was consumed. After some discussion, it was ...
7
votes
2answers
3k views

Removal of tetrabutylammonium from an organic reaction

I need to synthesize some organic compound for my Ph.D. research. Everything went OK during the synthetic route but got messed up at the very end. In my final step (once the final compound has been ...
1
vote
2answers
187 views

Drying solvents while taking care of purity

I need to dry some solvents like $\text{MeOH, EtOH, and DMSO} $ and I have to take care of purity of the solvents. These solvents are HPLC grade. I am interested in freezing point and boiling point ...
5
votes
4answers
141 views

To heat or not to heat; distillation?

One of the questions in a recent past paper I completed was: One way to make water from the reservoir suitable for drinking is by distillation. Describe how water is distilled. And I answered ...
1
vote
1answer
697 views

How can I isolate glycolic acid from sugarcane juice?

This beginning of a bachelor thesis uses ethylene glycol as a catalyst in the isolation of glycolic acid. I can't find the rest of the article (it ends in the middle of the description) to find out ...
3
votes
1answer
363 views

Textbook chemistry vs Real life chemistry and impurities

Long ago when I took chemistry courses in high school and lower, chemistry seemed so simple and elegant. All equations and exercises involved pure elements, pure compounds, with a very clean ...
4
votes
1answer
2k views

Mechanism of protein precipitation with TCA

In practice, TCA (trichloroacetic acid) is widely used for quantitative protein precipitation, but so far I have failed to discover the exact mechanism of TCA action. I highly doubt it's just the ...
0
votes
0answers
122 views

How to purify volatile haloalkanes prepared by Darzens halogenation?

We know that the Darzens method of substitution works on $S_n i$ and is considered the best method in terms of yield of product. Also the side products are $\ce{SO_2}$ and $\ce{HCl}$ so the ...
2
votes
0answers
2k views

How to prepare glacial acetic acid from sodium acetate?

What would be the most practical process to prepare glacial acetic acid from sodium acetate? I'm thinking to react the sodium acetate with an acid to convert the solution to acetic acid and sodium ...
1
vote
2answers
2k views

Dry Hydrogen Production

I am building a set-up to produce a controlled flow of dry hydrogen. I'm aiming for around 99.5 percent purity. Am I right in thinking a PEM cell and Deterite drying tube should be fine for this? Or ...
5
votes
1answer
616 views

Purification of Ethanol

In Vogel's organic book, they have mentioned that in the Lund and Bjerrum method of purification of ethanol, magnesium is added, which forms ethanolate. But they said to activate the magnesium first ...
3
votes
0answers
152 views

How can I purify ethanol from formic / boric / salicylic acid?

I need some ethanol pure and strong enough for technical purposes (fuel, solvent, cleaning agent, dissolving rosin for soldering flux, etc.). Food quality is not required though, denaturated one is ...
1
vote
0answers
668 views

How to crystallize out reaction mixture from DMF?

Reaction was carried out in DMF, and TLC shows that the reaction has completed. But how to separate reaction mixture i.e. product from DMF? Edit Steglich Esterification was carried out and the ...
3
votes
1answer
1k views

Recrystallization of two unknown compounds?

I managed to separate a binary mixture(in solid form) of two unknown substances into two individual solid compounds. For the separation, I used an acid-base extraction with dichloromethane, NaOH, and ...
5
votes
1answer
21k views

Why is crystalline aspirin washed with chilled water in the purification process?

Take as example this or even better this: Wash the crystals with 2-3 ml of chilled water. Why does the aspirin need to be cooled down? And why do we wash the aspirin with chilled water?
1
vote
2answers
469 views

Different techniques of distillations

I know that fractional distillation is used to separate two liquids that are miscible in one another and have close boiling points. However, I am really confused about vacuum and steam distillation - ...
6
votes
2answers
231 views

Removing titanium from tantalum crucible

I'm trying to remove titanium filling from a tantalum crucible for a high-temperature effusion cell. I've managed to get a majority of the material out with tweezers, but some remains and is ...
9
votes
1answer
761 views

Is it safe to condense water into a liquid nitrogen trap?

I'm trying to remove water from an imidazolium salt (i.e. dry the salt). However I want to know if it is safe to remove the water under vacuum. Is it safe to condense water into a liquid nitrogen ...
7
votes
1answer
1k views

What is the behavior of a Zwitterion during ion exchange chromatography?

We're interested in purifying a protein that has an azide moiety using ion exchange chromatography. Due to its unique structure, the moiety is a Zwitterion with a novel chemical behavior. My question ...