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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Selective halogenation of an alkane

Is it possible to selectively halogenate a certain position on an alkane chain, and also get a good yield? I understand that to form such haloalkanes, taking a different substrate other than alkane (...
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Condensation reaction between catechol and acetone

I was thinking of ways to synthesize 2,2-bis(dihydroxyphenyl) propane and I thought it could be made by a condensation reaction between dihydroxybenzene (catechol) and acetone in strongly acidic ...
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How would one favor the formation of p-TsCl over o-TsCl in the chlorosuflonation of toluene? [closed]

I found an old synthesis of $\ce{o-TsCl}$ that purportedly gives a yield of $85\%$ here and was wondering how, still using chlorosulfonic acid, I could favor the formation of $\ce{p-TsCl}$ instead.
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80 views

Sodium hydride 60% dispersion in mineral oil [closed]

I've got a bottle of sodium hydride 60% dispersion in mineral oil. It's not "in mineral oil" it's just powder with an oil coating. I'm using it in an inert reaction, is there a way to remove the oil?
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chitosan question [closed]

when chitosan is coated on the surface of iron oxide nanoparticles, are the amine groups of the chitosan pointed out?
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106 views

Solvent for reaction mixture

I'm looking for some suitable solvent for ether cleavage of Guaiacol (o-Methoxyphenol) using aluminium triiodide ($\ce{AlI3}$) with $\ce{DMSO}$. The original paper calls for using hot acetonitrile as ...
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158 views

How is bromothymol blue synthetised?

In a classical reaction, phenolphthalein is synthetised from phthalic anhydride and phenol with acid catalyst. When one uses substituted phenols, one obtains similar compounds (e. g. cresolphthalein, ...
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21 views

Simple synthesis of thiocyanates

Can sodium thiocyanate be synthesised by combining equimolar amounts of ammonia, sodium hydrosulfide and carbon dioxide in the presence of phosphorous pentoxide by the following reaction: NH3 + NaSH + ...
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129 views

What's the purpose of an ice bath when preparing a nitration mix from KNO3?

Most preparations for nitrocellulose from $\ce{(KNO3 + H2SO4)}$ mixture require the use of an ice bath during the process of dissolving $\ce{KNO3}$ into $\ce{H2SO4}$. Last time I did this I omitted ...
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62 views

Synthesis of the tetrachloroaluminate(III) anion

Looking for random chemicals, I found a reference on the anion and thought that it could be synthesised from common laboratory reagents: $$ \begin{align} \ce{2 Al + 2 NaOH + 2 H2O &-> 2 NaAlO2 ...
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134 views

What is the mechanism of this reaction?

I've been stuck with this for some time. I just don't see it. As the reactant is Pd(0), I think oxidative addition will happen to the bromine. Then I would say an insertion reaction happens. However ...
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81 views

Problem with synthesis of calcium formate

I just tried preparing calcium formate by adding $\ce{Ca(OH)2}$ to ammonium formate, but I observed no bubble formation and no smell of ammonia. Why doesn't calcium hydroxide, being a strong base, ...
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406 views

Mysterious precipitate in reaction of copper sulfate and calcium hypochlorite

So I can’t seem to figure this reaction out. I’m pretty new to chemistry and am still learning it in high school so please don’t think I’m stupid. I have reacted 2 solitons (copper sulfate) and ( ...
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291 views

Reference request on potassium cyanide production method

I kindly ask for a reference for the following claim about potassium cyanide, found at potassium.atomistry.com: It is also obtained by the action of a mixture of steam and nitrogen on potassium ...
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284 views

Copper (II) chloride reduction with Hydrogen gas

I've been looking into making pure copper (I) chloride, but using ascorbic acid is relatively expensive for me. I'd also like to avoid having water in any part of the synthesis to minimize the ...
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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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Have IH₃ and IH₅ already been synthesized?

I've seen a paper by Sikalov [1] that says that $\ce{IH3}$ and $\ce{IH5}$ should be observable. Has anyone actually tried to synthesize such molecules? References Sikalov, A. A. Hypervalent Halogen ...
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275 views

Why cobalt reacts favorably with nitrogen?

I used also iron, nickel, zinc, copper. However, cobalt gives the easiest and straight forward yield of nitrides (XPS and SAED verified). It is so easy to get cobalt nitride that I don't even have to ...
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180 views

Preparation of compounds using acetoacetic ester synthesis

I've been given the following exercise in organic chemistry, and I'm at a complete loss. The text book doesn't cover the subject at all. I have some knowledge of melonic ester synthesis. As an ...
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359 views

Reduction of amino acids to corresponding amino alcohols

I've stumbled upon an interesting article about reduction of amino acids and from there to reduction of L-valine to L-valinol using $\ce{LiAlH4}$ in THF. Article says that because of the cost of $\...
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92 views

Best method to increase the chain length of allyl to butane-1,2-diol [closed]

Best method to increase the carbon chain length of allyl. and also add 2 OH carbon after reducing double bond give (S)-4-R-butane-1,2-diol and (R)-4-R-butane-1,2-diol . R= Any Ak, Cb, Cy, Hy
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415 views

How to obtain sodium oxide from sodium chloride?

Under what conditions can $\ce{Na2O}$ be made from $\ce{NaCl}?$ I know $\ce{NaCl}$ doesn't oxidise under normal ambient conditions, but in the presence of what temperature and pressure ranges is this ...
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method of separating product and conserving the catalyst

I'm looking for a way to separate reaction product of iodobenzene with ethyl 2-methyl-3-oxopentanoate in 1,4-dioxane (toluene is an alternative as a solvent). The catalyst being used is Pd2(dba)3 with ...
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521 views

Obtaining mercury from mercury(II) nitrate

I was thinking about obtaining mercury from mercury(II) nitrate. Is it possible? I've tried putting chunks of Fe into it, I've got the logic from the voltaic table (where Fe is on the left side of Hg, ...
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61 views

Reference request on formate potash process

Wikipedia article on Potassium Formate mentions a so-called "formate potash process" for production of potassium, presumably referring to elemental metal. Concise encyclopedia chemistry by Mary ...
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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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Methylammonium lead(II) iodide perovskites in bulk form

I am trying to obtain $\ce{(MA)PbI3}$ as a bulk powder using lead(II) iodide and methylammonium iodide as precursors. I have not yet tried simply mixing the two in methanol/ethanol and removing the ...
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53 views

Hydroxy Protecting Groups that are not Cleaved Under Acidic Conditions

I am currently designing a synthesis requiring the use of hydroxy protecting groups. The problem I am having is that the protecting group must be able to survive highly acidic conditions. I would have ...
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264 views

Phosphoryl bromide reaction with benzoic acid

I am trying to find out how $\ce{POBr3}$ reacts with $\ce{-COOH}$ group (benzoic acid to be specific). I found that it performs an elimination reaction with alcohols to give alkenes. I have also seen ...
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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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What is the largest one step radical cyclization ever achieved?

When I was an undergrad, roughly around 2005, I took a grad level class that covered various topics in advanced organic synthesis. I don't remember much clearly from the class, but one thing that I ...
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194 views

Balanced equation for Schweizer's reagent production?

In Thompson's Illustrated Guide to Home Chemistry Experiments the chemical formula for Schweizer's reagent is represented as $\ce{[Cu(NH3)4](OH)2}$ (although Wikipedia represents it as $\ce{[Cu(NH3)4(...
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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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Molar ratios not leading to complete reaction in Schweizer's reagent production

In my home lab, I've reacted $\ce{Cu(OH)2}$ with aqueous ammonia to produce Schweizer's reagent. However, I'm surprised by the amount of ammonia required to react with this amount of $\ce{Cu(OH)2}$. ...
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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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586 views

Making aspirin without acetic anhydride

I want to make aspirin. Normal method is to react salicylic acid with acetic anhydride, but it is extremely hard to find acetic anhydride. How may I synthesize aspirin with acetic acid and salicylic ...
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108 views

Why is t-BuOK necessary for this synthesis?

1-chloro-2-methylpropane --> 2-chloro-2-methylpropane. My understanding is that an E2 reaction produces two types of alkenes, the major product for non-sterically hindered bases is the more ...
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130 views

How to dissolve PLA/PCL/PMMA?

I have a research about electrospun membrane synthesis where I dissolve PLA pellets in chloroform:methanol (3:1) for 3 hours and also PCL pellets in chloroform:methanol (3:1) for 3 hours too. Another ...
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666 views

How to convert Mn2O3 to Mn3O4?

I was preparing $\ce{Mn3O4}$ but it was when characterized by XRD, a $\ce{Mn2O3}$ phase existed. Now how can I convert $\ce{Mn2O3}$ to $\ce{Mn3O4}$?
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154 views

Why is it ill advised to eat the solid aspirine formed from salicylic acid + acetic anhydride

In the laboratory notes it is indicated that it is ill advised to eat the solid formed from this experiment. An esterification reaction, in which salicylic acid is treated with acetic anhydride. If ...
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34 views

How can the free amino acid B be enantioslectively synthesitzed?

I would like to know how this reaction actually works. I think its an ring metathesis, espececially with the Grubbs catalysator II. But I dont know how to this reaction examole really works especially ...
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Shi Epoxidation Issues - Any help would be appreciated

As part of my PhD project, I'm currently looking into running a Shi Epoxidation reaction. The first step is to reproduce the current literature on this reaction by using trans-stilbene as my substrate....
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135 views

Synthesis of copper selenide

If I react selenium powder with copper chloride powder above the melting point of selenium (221 °C), will I end up with a chunk of copper selenide, with the chlorine given off as gas, or will I lose ...
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Why is tert-butoxide often used in elimination reactions when it is not necessary?

I understand that tert-butoxide is used to favor the Hofmann product in elimination reactions due to its steric bulk (and thus inability to abstract a proton in a more substituted position); however, ...
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128 views

Preparation of 3-ethylpentan-3-ol

Is it possible to use CI3TMS (a carbon with three iodo groups and a trimethylsilyl protecting group) and three equivalents of an ethyl grignard reagent to prepare 3-ethylpentan-3-ol? By deprotecting ...
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125 views

Preparation of Effexor

I take venlafaxine (Effexor) as medication, and having wrapped up 2 semesters of Organic Chemistry I thought it might be fun to design a synthesis for it. A picture of venlafaxine: I came up with the ...
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Synthesis of potassium trioxalatocobaltate(III) trihydrate

I've synthesized the compound potassium trioxalatocobaltate(III) trihydrate and for it I have two reaction equations. One of them is: $$\ce{CoCO3 + 3K2C2O4.2H2O -> K2[Co(C2O4)3] + 2CO2}$$ and the ...
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What is the most convenient way to prepare ferrous oxide (FeO) in the laboratory?

The Wikipedia page for ferrous oxide states that $\ce{FeO}$ can be prepared by the thermal decomposition of iron(II) oxalate, with the following reaction: $$\ce{FeC2O4 → FeO + CO2 + CO}$$ And that ...
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73 views

Is it possible to synthesize permanganate electrochemically?

I have been researching the production of peroxy acids and other strong oxidizers. I was wondering if it's possible to produce permanganic acid if I were to cast an anode containing Manganese Dioxide ...
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262 views

How to make aluminium monostearate?

Can I make aluminium monostearate $(\ce{C18H37AlO4};$ $\pu{344.472 g mol-1})$ by reaction between stearic acid $(\ce{C18H36O2};$ $\pu{284.484 g mol-1})$ and aluminium hydroxide $(\ce{Al(OH)3};$ $\pu{...

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