Questions tagged [synthesis]
Synthesis is a purposeful execution of chemical reactions to obtain the desired product. Applies to long and complex natural product syntheses as much as to short one or two-step syntheses. This also covers synthetic problem sets and retrosynthetic analyses.
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Can 4-pyridones be synthesised analogously to 2-pyridones?
I understand that 2-pyridone derivatives can be synthesized by oxidizing an N-methyl pyridinium salt with $\ce{[Fe(CN)6]^3-}$ under basic conditions. Can a similar method be used to produce 4-...
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What aspects of a molecule's chemical makeup determine which portions of it will react?
Is there a specific way to know how two or more arbitrary molecules will react?
An example that prompted this question: $\ce{(HOC6H4)2CMe2 + 2 NaOH → (NaOC6H4)2CMe2 + 2 H2O}$ (from here). How can ...
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preparation methods of nicotinoyl glycine
How can we prepare nicotinoyl glycine from nicotinic acid ?Is that possible by reaction between nicotinic acid and glycine?
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Palladium coupling reactions and purification
I tried to synthesize 2-(6-fluoropyridin-3-yl) acetic acid from 5-(Chloromethyl)-2-fluoropyridine using Pd(OAc)2/PPh3 catalyst,Na2CO3 and DCC. I eluted my product on TLC with Ethyl acetate/hexane/...
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Could a de-commissioned synthetic ammonia plant be adapted for use in removing CO2 from the atmosphere (DAC)?
I was prompted to ask this question by viewing a disused $\ce{NH3}$ plant in the harbour near where I live.
Like many it functioned using a methane feedstock from a natural gas find off the coast. I ...
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Why does hydrogen peroxide decompose during the oxidation of an aryl amine to and nitroarene (rt) and what are the possible overoxidation products?
Small scale:
I attempted the oxidation of an aryl amine (2-amino-6-bromonaphtalene) to the nitroarene using hydrogen peroxide (ArNH2, H2O2, MeCN (15 mL as solvent). After trying it on small scale (0.1 ...
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What is this gel byproduct of acetylsalicylic acid recrystallization?
I did a very simple acetylsalicylic acid synthesis from salicylic acid and acetic anhydride (with phosphoric acid as a catalyst). After rinsing, filtering and drying the product I dissolved it in ...
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Why did this synthesis of Aspirin fail?
I tried to synthesize acetylsalicylic acid(aspirin) by the method below. However, I definitely failed and got something unknown.
The method used was:
Add 2.5 g of salicylic acid(about 2494 mg), 3.0 ...
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Synthesis of 1-ethylcyclohexane-1,2-diol from cyclohexylethene
Here's my synthesis:
HBr
NaEtO
OsO4/NMO
But the problem is that for step 2, there are 3 possible alkene locations, with all of them having 3 substituents, so I would have all 3 forming (although 2 ...
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Amidine synthesis from nitrile and dimethylamine using n-Buli as a base
I am making LiNMe2 using n-Buli (5.5 equiv.) and dimethylamine (5.0 equiv), -15 ºC, dry THF and under nitrogen atmosphere.
I have been doing the reaction and I can observe conversion of starting ...
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TMSiBr and Oxalylchloride for ester cleavage
I am wondering what is the advantage of using TMSiBr do perform an ester cleavage in comparison to perform chlorination first for example with oxalylchloride or thionylchloride and than add water?
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Esterification of phosphonic acid chloride is working with isoprenol but not with prenol
I am performing an esterfication reaction between an activated phosphonic acid (chloride) and a series of alcohols. Until now, I was not able to make the reaction work with prenol, while isoprenol is ...
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Avoid triethylphosphate as a side product during P-C-P coupling reaction with diethylchlorophosphate with LDA
I have a reaction in which I perform a deprotonation of an acidic proton at a phosphate and later do a P-C-P coupling. The coupling partner is diethylchlorophosphate. Deprotonation is performed with ...
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Is it possible to prevent elimination during Diels Alder reactions using Danishevsky's diene (or variants)?
Are there examples of keeping the methoxy group and then using it to perhaps do radical chemistry without eliminating to the enone?
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Cause and Prevention of Palladium Mirror in Stille Coupling
I am conducting some monomer and polymer syntheses using Stille coupling or other palladium-based coupling. I usually use the combination of $\ce{Pd_2(dba)_3}$ and $\ce{P(o-tol)_3}$ in Stille coupling,...
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Erythritol oxidation using acidified KMnO4
I have recently experimented with erythritol oxidation my primary aim was to make glyoxal. However regarding the nature and structure of erythritol several other side-products were also observed one ...
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Functional groups in graphene oxide
There is already a large number of literature on graphene oxide stating that the number of epoxy groups is quite similar to the number of ethyl groups. However, I was wondering if the number of ...
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Does the metal complexing of crown ether influence its reactivity?
I am conducting a SN2 reaction experiment with 1-aza-18-crown-6 and bromide compound. I used 1 equivalent of bromide compound and 1.1 equivalent of aza crown, but in the TLC plate the aza crown spot ...
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Does the Darzens reaction work with an alpha-chlorocarboxylic acid and an aldehyde?
Is it possible that a reaction of an alpha-chlorocarboxylic acid with an aldehyde work for the Darzens reaction to produce an epoxide (with NaOH as the base, and H3O+ workup)?
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Mechanism for reaction of beta-ketoacid with AcONa, AcOH with heat
I am unsure of how to go about designing a mechanism for the following molecule's reaction with AcONa and AcOH with heat.
I thought perhaps it may work as a cyclisation reaction, forming an ether; or ...
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Recovery of precipitated polymer
I have recently newly synthesized the polymer. Based on its structure I tried to precipitate its concentrated solution in dichloromethane by dropping it into methanol. It seemed to work. The methanol ...
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Preventing solvent evaporation for small scale synthesis
I have been conducting an organic synthesis with quite expensive starting material, so whenever I setup the reaction I only use 0.1 g of starting material. I use 4 mL of toluene to adjust the ...
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Amides from carboxylic acid and ammonia?
Would it be possible to synthesize amide by simply reacting carboxylic acid with ammonia and then driving off water at higher temperatures? Or would ammonia be also driven off in the process?
Google ...
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Mechanism of this addition-elimination process
In Part 1 of the synthesis of Maoecrystal V (found on synarchive), the last step subjects a $\ce {\alpha, \beta}$-unsaturated ketone to $\ce {I2}$ and pyridine, as shown below:
I am wondering what is ...
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Accidental hydrolysis of tert-butyl chloride
Yesterday, I performed the synthesis of tert-butyl chloride from tert-butyl alcohole in my practical organic chemistry class. However, I only obtained a relatively low yield of about 30 %. Since I ...
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Reason for adding TFAA in this synthesis pathway?
I have included a short part from a synthetic pathway from: https://synarchive.com/syn/112
$\ce{Mg3N2}$ reacts with $\ce{MeOH}$ to liberate $\ce{NH3}$ which I believe is used in nucleophilic ...
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Differences in activated manganese dioxide synthesis
I've looked into preparations of activated manganese dioxide for some time now, and what confused me is the contrast between the original Attenborough method and some of the alternatives.
A solution ...
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Problem about TLC solvent and staining
I am conducting an organic synthesis involving 1-aza-18-crown-6-ether. I tried TLC, but they didn't work well. I have tried: (1) hexane+ethyl acetate in various ratio, (2) dichloromethane:methanol=3:1,...
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Can you develop algorithms to predict synthesis of peptides?
This may be a very foolish question, but do (complex) algorithms exist to predict the steps and materials involved (or therefore different options and paths) in synthesis for the given input of for ...
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Procedure for laboratory synthesis of tertiary amines [closed]
I am having difficulty finding a procedure for making tertiary amines in the lab, any is fine but I am specifically interested in tributylamine.
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Alkylation of enolates using tertiary halide
I was recently studying the alpha alkylation of enolates using LDA followed by subsequent treatment with primary halides to give the product.I was wondering what happens with teritary halides. My ...
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Chemically producing sodium metal from magnesium
Anyone with experience making sodium metal ($\ce{Na}$) with the following process? Reactants: $\pu{14 g}$ magnesium powder, $\pu{20 g}$ sodium hydroxide; Catalysts: $1$ to $\pu{2 g}$ menthol crystals; ...
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Is it possible to add R chain that contains a carbonyl (ketone) to the alpha carbon?
I'm trying to synthesize 2‐(3‐oxobutyl)cyclohexan‐1‐one from cyclohexanone:
I thought about LDA, then adding an R group that has a ketone. Is that possible? As far as I know, we can add halogen or ...
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How to efficiently weight DCC (N,N'-Dicyclohexylcarbodiimide)?
I have to run a reaction using N,N'-Dicyclohexylcarbodiimide and at room temperature, it is solid, but it's very hard to weigh. I know its melting point is around 40 degrees. Is it better to melt it ...
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How is lapping slurry made?
I've recently gained an interest in the whole topic of lapping and the creation of flat surfaces.
Lapping is done in different ways, but the one I'm interested in is essentially just rubbing 2 ...
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Does DIBAL-H reduce alcohol?
Does DIBAL-H reduce alcohol? I was reading an article by Rentsch and Kalesse [1] and I came across this reaction, but could not figure out how the final compound is formed:
Reference
Rentsch, A.; ...
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Reaction analogous to burning that causes cooling rather than releasing heat [closed]
Is it physically and chemically possible to design both a gas and a solid substance, such that there would be a technologically feasible initiation of a chain reaction analogous to the spark that ...
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How concentrated does sulfuric acid need to be for nitric acid synthesis (H2SO4 + nitrate salt distillation)?
So I have a home lab setup and recently found myself in need of some nitric acid. I could just buy some, but I thought it would be a useful exercise to make my own. I have plenty of nitrate salts ...
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Definition of throughput
I wonder what's the exact meaning of throughput in chemistry synthesis, eg. in organic synthesis or production of pharmaceutical products. For instance, what are their units? How are they measured?
I'...
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Conversion of Erythrosine to Fluorescein
I am a home-chemist and I love dyes. I recently got my hands on sodium salt of erythrosine (tetra-iodinated fluorescein). I want to convert erythrosine to fluorescein. I speculate that using dilute ...
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Dispersity of synthetic DNA [closed]
Recently I was reading an article about DNA nanostructures and I was wondering--
I know that DNA in living systems is monodisperse, but when we make DNA synthetically, is it truly monodisperse or ...
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Synthesis of Schiff Bases in Aqueous Media
The paper https://www.hindawi.com/journals/jchem/2013/909217/ describes a possibility to synthesize salicylaldehyde-based Schiff Bases using water as a solvent. Yields shown for the microwave-assisted ...
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What is the best way to make a substantial amount of soot in a high school laboratory?
I need to make about 50 grams of soot (carbon black particles) in a high school laboratory. What would be the best way to do this?
The purpose of needing 50 grams of soot is because I would like to ...
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L-lysine acetate synthesis
Is it possible to synthesize L-lysine acetate in the following steps? First, mix L-lysine HCl with an excess of NaOH and just enough water so that the total water in the product is enough to solve all ...
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Source of highly nucleophilic iodide [closed]
What is be the best commercially available source of highly nucleophilic iodide in non-polar solvent? Solvents used are cyclohexane, benzene, chlorobenzene.
I can get ahold of bromide quaternary ...
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Fischer Esterification of the Unsaturated 3-Butenoic Acid with Methyl Alcohol
I am attempting to perform a Fisher esterification of 3-butenoic acid (vinyl acetic acid). I believe that this should theoretically work and not disturb the unsaturated region of the molecule, but I'm ...
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Reaction with ethyl chloroacetate and potassium carbonate
I am carrying out a reaction using ethyl chloroacetate, potassium carbonate in acetone for a compound containing $\ce{-NH}$ group. So, the substitution will be at $\ce{-NH}$ position.
I have tried ...
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How to get rid needle clogging on electrospinning of PLA/PCL/PMMA/Collagen?
For my thesis research, I dissolved PLA and PCL in chloroform: methanol (3:1), PMMA (350.000 MW, 13 wt%) in acetone, and collagen in acetate acid--and then, I mixed them together. The problem is when ...
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Selective Esterification of Amino Acid
I am going to prepare tert-butyl protected threonine. I was going for the classic esterification methodology which is acid catalyzed (sulfuric acid) esterification under reflux of tert butyl alcohol + ...
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Organometallic Synthesis: Cp2Ti(I)Me from TiCl4
I've been working on this synthesis question for a couple days but I'm a little stuck. The question is:
Using only $\ce{TiCl_{4}}$, $\ce{NaCp}$, $\ce{PhLi}$, $\ce{MeI}$, and $\ce{EtMgBr}$, ...
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