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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Synthesis of polypropylene

So, I have two questions regarding the synthesis of polypropylene: I have tried looking everywhere but couldn't find a detailed mechanism for the termination step of the synthesis of polypropylene (...
Guy Weizman's user avatar
5 votes
2 answers
148 views

Synthesizing Cyclotetrazane from Hydrazine and Diazene?

Could cyclotetrazane — a compound with nitrogen atoms arranged in a square configuration — be synthesized? A hydrogen atom would be bonded to each vertex (nitrogen atom): Could cyclotetrazane be made ...
Nitrogen-8's user avatar
2 votes
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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/...
Ella's user avatar
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Electrophilic fluorination power: selectfluor vs NFSI

I want to fluorinate the methylene hydrogens between an aryl group and a phosponate ester. The reaction is similar (not identical) to this one: For some reason on the literature people are using very ...
raptorlane's user avatar
1 vote
0 answers
32 views

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 ...
RetroFan's user avatar
3 votes
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63 views

With two reagents common on Mars, fluorite and CO2, how would I produce carbon tetrafluoride?

The hypothetical terraforming of Mars would require the heating of the atmosphere. A commonly suggested method is the in-situ production of fluorocarbons, powerful greenhouse gases. For example, ...
Galerita's user avatar
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What type of sugar is produced A. Tutton's Paper on the Synthesis of Glucose?

https://www.nature.com/articles/037007b0 At the end of all the chemical reactions, a sugary substance is identified by what sugar it is is not specified so I would like to know what it may be. (On a ...
Curiousmind's user avatar
2 votes
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34 views

Synthesize pivaloyloxymethyl ester, but with a substrate that is a terrible nucleophile

I want to synthesize an pivaloyloxymethyl ester from a fluorophosphonic acid. The idea is, to make a compound cell permeable that than be cleaved in the cell by enzymes. Apparently, the acid is a very ...
raptorlane's user avatar
4 votes
0 answers
41 views

Why cool a reaction down when adding reagents if you're only going to reflux subsequently?

I've seen several procedures using thionyl chloride (SOCl2) to make an ester, where the first step is to add the thionyl chloride to the reagent/solvent on ice or subzero temperature, followed ...
sat0ri's user avatar
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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 ...
The Red Man Jolan Bonelli's user avatar
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What is the difference in reactivity between the various borates (trimethyl, triethyl, triisopropyl borate) to form boronic acids?

For the transformation of 1,3-dibromobenzene to bromobenzene boronic acid, different groups use different boration reagents namely trimethylborate, triethyborate and triisopropylborate). The reaction ...
The Red Man Jolan Bonelli's user avatar
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31 views

Need Suggestion for Picking the Right Solvent for Column Chromatography

I've completed my reactions, and based on the stoichiometry and TLC analysis, I think my mixture should contain 3-4 compounds: Ethyl gallate (my product) Gallic acid (the reagent/starting material) ...
Jonathan's user avatar
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4 votes
0 answers
227 views

Exchange of Fluorine to Oxygen for Fluorophosphonic acid by silylating agents or other methods?

[Warning, long post!] Dear all, I am confronted with a seemingly easy transformation. I want to remove a fluorine atom at a fluor phosphonic acid salt. The usual method to achieve this is the basic ...
raptorlane's user avatar
1 vote
1 answer
112 views

How does the following cyclization reaction work?

The following is a reaction from a school provided lab manual. However, I am unable to find anything similar to the cyclization reaction taking place. All of the reactions I have found online make use ...
Marethyu's user avatar
2 votes
0 answers
27 views

TMSBr and 2,4,6 Collidin in Acetonitrile leads to white precipitate

I want to hydrolyse a phosphonic acid ester with TMSBr. I think this reaction works only with the addition of base. Without base, the product in my specific case is prone to deterioation due to acid ...
raptorlane's user avatar
1 vote
0 answers
37 views

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 ...
Thomas's user avatar
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2 votes
0 answers
104 views

Removing DCC and its by-product from Steglich Esterfication

In my small research, I want to synthesize 3 alkyl gallates (ethyl gallate, butyl gallate, and hexyl gallate), and here's my overall reaction using Steglich esterification): However, from reading ...
Jonathan's user avatar
  • 117
7 votes
2 answers
580 views

Question about the differences of white and grey NaH properties

We are having some problems with the next reaction in our lab. As you can see, is the sulfonylation of an indole in which we use NaH (60% dispersion in mineral oil) as a base. This reaction goes with ...
Alicia's user avatar
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4 votes
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Hydrolyse a fluorophosphonic compound / Which protective group strategy can I use for phosphonate esters to access the free acid after a reaction?

I have a synthetic problem in my PhD thesis, in which I synthesize a phosphonate ester. To be more precise, it is a phosphonofluoridic compound. In my specific case, the fluorine attached to the ...
raptorlane's user avatar
0 votes
0 answers
75 views

Steglich Esterification in Alkyl Gallates

Based on my research (reading some articles), some alkyl gallate syntheses used Steglich esterification instead of the usual esterification (Fischer esterification). The reason why Steglich ...
Jonathan's user avatar
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2 votes
2 answers
209 views

Should I remove inhibitor from methyl acrylate?

I need to run multiple aza-Michael additions of methyl acrylate with various amines (dimethylamine, benzylamine, phenylethylamine, aniline, etc.) in order to get the bis-ester. I was wondering if the ...
Matt's user avatar
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33 views

Breakdown of addition polymers

We know that condensation polymers can be broken down by hydrolysis with the elimination of small water molecules. Then what about addition polymers? How can they be broken down into their monomers? I ...
Freeby Freeby's user avatar
-3 votes
1 answer
69 views

Synthesizing "Methyl 2-(2-oxopyrrolidin-1-yl)-2-phenylacetate" [closed]

I am a chemistry student, here I mapped out the steps one might take to synthesize Methyl2-(2-oxopyrrolidin-1-yl)-2-phenylacetate, a piracetam dirivitive. Please add any steps I might be missing and ...
Tom's user avatar
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0 answers
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Advise on performance vs cost of the Berkland-Eyde Process for direct synthesis of Nitric Acid from atrmospheric air

I am new to chemistry, having gone down an electronics route in my career, so I decided to pick up where my 'O' levels ended (many years ago) and make a better understanding of the topic a sort of ...
Jay M's user avatar
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0 answers
51 views

Methanisation in the Haber Porcess

I've been reading up on the Haber process lately. In one such industrial case of ammonia synthesis, hydrogen is created through steam reforming, which creates some carbon monoxide. As the reaction ...
Jay Chen's user avatar
2 votes
0 answers
79 views

What is the product and mechanism of reducing a cyclohexanone derrivative with LAH?

I've been trying to figure out the product and mechanism of the reaction pictured below for a while now: I'm fairly sure that the first step is the reduction of the ketone by LAH, which results in a ...
HWABAG's user avatar
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3 votes
0 answers
102 views

Hydrolyse Phosphonate diester to free phosphonic acid under relatively mild conditions?

I want to hydrolyse a phosphonic acid diethylester to the corresponding free phosphonic acid. In the literature, it is described, that usually strongly basic or acidic conditions are utilized to ...
raptorlane's user avatar
1 vote
0 answers
119 views

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 ...
user139437's user avatar
-3 votes
1 answer
184 views

Production of sulphuric acid

To my knowledge, sulphuric acid is produced by complex industrial processes like contact process. The following structure shows a sulphate ion. I wonder why sulphuric acid cannot be produced through ...
Freeby Freeby's user avatar
2 votes
0 answers
77 views

Reduction of benzylic alcohol and halide using H2 and Pd

I am studying drug synthesis, and I found some examples that uses $\ce{H_2}$ and Pd/C or Pd/$\ce{BaSO_4}$ as catalytic hydrogenation reagents for reduction of alcohol or halide in benzylic position. ...
Krang Lee's user avatar
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2 votes
0 answers
50 views

Degradation of 4-MeO-Tetrahydrocarbazole

I recently synthesized 4-Methoxy-Tetrahydroxarbazole from 4-MeO-Phenylhydrazine and Cyclohexanone. The product had a off-white color directly after synthesis but was brown after standing over night at ...
arausch's user avatar
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1 vote
0 answers
54 views

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 ...
Toast's user avatar
  • 11
0 votes
0 answers
67 views

Find the missing chemical structures in the reaction sequence

I came across the following question, where a set of reagents are used, starting from a carbohydrate derivative. I understand that this is some total synthesis reaction, but I cannot find which one. ...
Cyclopropanol's user avatar
5 votes
1 answer
238 views

Selective formation of enolates

I saw the following reaction on Modern methods of Organic Synthesis by Carruthers. The reaction is about the selective alkylation of trimethylsilyl enolates, and is shown below. However, I have some ...
Cyclopropanol's user avatar
1 vote
0 answers
50 views

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 ...
Bree's user avatar
  • 11
-1 votes
3 answers
113 views

Can any compound form into an amorphous solid?

I am curious whether it is possible or not to make any solution of a specific compound into a crystal lattice or into an amorphous solid? I know that crystals form under specific conditions but seem ...
Brian Blumberg's user avatar
1 vote
0 answers
53 views

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?
raptorlane's user avatar
1 vote
0 answers
43 views

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 ...
raptorlane's user avatar
-4 votes
1 answer
99 views

Reaction of eugenol with concentrated hydrobromic acid in the presence of gaseous hydrogen bromide [closed]

DISCLAIMER: I am not using any of this information to commit a crime, my university has a license from the relevant authorities to investigate clandestine chemical procedures. We are investigating an ...
user1754943285's user avatar
1 vote
0 answers
33 views

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 ...
raptorlane's user avatar
5 votes
0 answers
44 views

Specific question about the total synthesis of B-12

In the process of synthesizing B-12, Woodward & Co. produce an intermediate thioether they refer to as Type I. "Type I because we found early in working with these substances that they were ...
GMoss's user avatar
  • 311
2 votes
2 answers
316 views

Are these reactions in synthesis of melamine correct?

I found the Wikipedia article for melamine to be incorrect in "synthesis and reaction" section; so I decided to edit it. But on the other hand I'm not sure my assumption to be correct that ...
Walter Heisenberg White's user avatar
2 votes
0 answers
107 views

Alternative synthesis for LK-99 proposed room-temperature superconductor

This is probably not the best place to post this, but I'm posting in case it might reach the right people who could give this a try. The current synthesis for the proposed LK-99 superconductor is a ...
MichaelK's user avatar
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2 votes
1 answer
40 views

Production SnO2 nanoparticles through chemical co-precipitation method: chemical equation of the reaction

In this paper, the production of $\ce{SnO2}$ nanoparticles through the chemical co-precipiation method is described using $\ce{SnCl2·2H2O}$ as a precursor. According to their experimental section, $\...
user21390097's user avatar
2 votes
2 answers
322 views

How do I synthesize salicylic acid?

I'm looking to synthesize salicylic acid in my school laboratory for an investigatory project. The Kolbe's reaction looks promising: Any suggestions on where to get the $\ce{CO2}$ from? Will the ...
Aditya Kumar Panda's user avatar
0 votes
1 answer
320 views

Magnesium chloride to citrate conversion (reaction/synthesis)

How would one prepare magnesium citrate from magnesium chloride and citric acid? Will it work if I just heat a mixture of magnesium chloride and citric acid in water? I'd expect HCl to vaporize off. ...
Mister Sir's user avatar
0 votes
0 answers
128 views

Color change when heating organic compound

I did just attend a lab class where I should synthesize 3,6-dibromo- N-propylcarbazole from N-propylcarbazole by bromination. Once, the bromination was over the color of the reaction content was ...
maniboy's user avatar
3 votes
0 answers
87 views

How does the synthesis of [18]annulene proceed stepwise?

Finding good literature on the synthesis of [18]annulene is challenging, as most sources are well old and quite archaic, so I was hoping some explanation in regard to the mechanism of synthesis. My ...
Evamentality's user avatar
2 votes
0 answers
91 views

Protecting Thiol group in presence of alcohol

What protecting group can I use that will protect the thiol in the presence of an alcohol? Is there a set of conditions, or a group that I can use that is selective to the thiol over the alcohol? I am ...
Maya H's user avatar
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1 vote
0 answers
35 views

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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