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Reusable fluorescent photocrosslinked polymeric sensor for determining lead ions in aqueous media


22 Dec 2016

Excellent method. Minor adjustment will make it even better

Summary:

A polymeric film as fluorescent sensor for detection of Pb2+ in aqueous solutions, synthesised from 1-vinylimidazole, poly(ethylene glycol) diacrylate and trimethylolpropane triacrylate has been described. The manuscript also describes the...

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Synthesis, characterization and DFT study of oxorhenium(v) complexes incorporating quinoline based tridentate ligands


22 Dec 2016

Good work, the basis set choice can be better

Summary:

The article presents the synthesis and characterization of two mononuclear Re(V) complexes. DFT and TD-DFT methods were employed for exploring the electronic structure and absorption spectra. Furthermore, the complexes were also tested for...

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Rapid determination of trace level copper in tea infusion samples by solid contact ion selective electrode


22 Dec 2016

Should include Mn & Al data for clarity

Summary:

A new copper selective solid-state electrode based on o-xylylenebis(N,N-diisobutyldithiocarbamate) ionophore has been described. It has been developed for selectively measuring the copper levels found in the tea infusion samples. Robust, cheap...

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Tetraalkylammonium salts in heck-type reactions using an alkali metal hydrogen carbonate or an alkali metal acetate as the base


19 Dec 2016

Seminal paper for phase-transfer Heck-Mizoroki cross coupling

A pinacle reaction of the synthesis required the cross coupling off a two highly heteroatom functionalised fragments, the use of traditional Heck conditions, such as palladium (II) acetate, triphenyl phosphine and triethylamine afforded poor yields and...

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Stereocontrolled construction of the trans-tetrahydrofuran units in Annonaceous acetogenins


19 Dec 2016

Experimental not reproducible as written

Procedure for synthesis of intermediate 2 was repeated three times at identical scale and reaction conditions as described and then modified. When followed exact same procedure as-written (12 hours), desired compound was obtained in 14% yield (confirmed by...

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Stereoselective Synthesis of 3-Hydroxyproline Benzyl Esters fromN-Protected β-Aminoaldehydes and Benzyl Diazoacetate


19 Dec 2016

Adaptations Necessary to Improve Published Syntheses

This review addresses the published preparation of compound 10c as listed in JOC 69, 4361 (2004).  The stated preparation utilizes the inexpensive, commercially available diol, 6c.  The preparation begins by combining the diol with one equivalent of TESCl in...

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O-(diphenylphosphinyl)hydroxylamine: preparation and some characteristic chemical reactions


19 Dec 2016

Adequate Synthesis; Improved Preparation Has Been Reported

This reaction was repeated to prepare O-diphenylphosphinyl hydroxylamine as this compound was reported to be a "less explosive" electrophilic aminating agent.  Note:  a recent improved preparation has been reported.  (DSC measurements of the isolated compound...

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Structural and conformational studies of 2-phenyl-1,3,2-diaza- and -dioxaboracycloalkanes


19 Dec 2016

Experimental Details

t-Bu amine (50 mmol) and methyl acrylate (50 mmol) were dissolved in MeOH (10 mL) and stirred overnight under nitrogen.  The secondary amine was isolated by Kugelrohr distillation after the MeOH had been removed by rotary evaporation.  The purified material...

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Three new mononuclear group 12 complexes with benzimidazole


15 Dec 2016

Reproducible but very routine work

Summary:

This paper describes the synthesis of three iso-structural Zn(II), Cd(II), and Hg(II) complexes with 1-benzyl-2-phenyl-1H-benzimidazole (BPB). Single crystal X-ray determination of CdBPB and HgBPB were done along with Structural analysis of ZnBPB...

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8-Dioxane ferra(III) bis(dicarbollide): A paramagnetic functional molecule as versatile building block for introduction of a Fe(III) centre into organic molecules


14 Dec 2016

Very useful paper for niche applications using metallacarboranes

Covalent attachment of 1,4-dioxane to beta born of ferracarborane sandwich complexes which can be easily outfitted with many organic functional groups. Procedure worked as reported, with moderate yields of 60-70%. Higher yields were achieved at smaller scales...

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Grindstone chemistry: protic ionic liquid-substrate tuned green synthesis of 1,2-disubstituted and 2-substituted benzimidazoles with outstanding selectivity


14 Dec 2016

Innovative, but better methods known

Summary:

An efficient and environmentally benign method for synthesis of 1,2-disubstituted and 2 substituted benzimidazoles has been described. Although previous methods are available in literature for synthesis of such compounds, the ease of operation,...

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An efficient green protocol for the synthesis of 2-aryl substituted benzothiazoles


14 Dec 2016

Good approach - less yields. Better methods reported already

Summary:

This paper reports the synthesis of 2-arylbenzothiazoles via cyclocondensation of 2-aminothiophenol with various aldehydes. Polyethylene glycol-400 (PEG-400) has been used as both solvent and catalyst for the process. The procedure applied, is...

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Relative Stability of Mixed [3 + 1] Tc and Re Complexes:  a Computational and Conceptual DFT Study


14 Dec 2016

Innovative study, but can be improved

Summary:

This paper describes the conceptual density functional studies on (3+1) complexes of both Re(V) as well as Tc(V). The tridentate ligands have been varied in order to study the effect of the various combinations of N, O and S chelating sites on...

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Synthesis, Characterization, and Catalase Activity of a Water-Soluble diMnIIIComplex of a Sulphonato-Substituted Schiff Base Ligand: An Efficient Catalyst for H2O2Disproportionation


09 Dec 2016

Good experimental, though extended rxn time beneficial

This paper describes synthesis, characterization, and catalase activity of a water-soluble diMn(III) complex of a sulphonato-substituted Schiff-base ligand. DiMn(III) complex is highly efficient to disproportionate hydrogen peroxide in basic aqueous solutions...

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An Efficient Method for Solution-Phase Parallel Synthesis of 2-Quinoxalinol Salen Schiff-Base Ligands


09 Dec 2016

Excellent reproducibility, some improvements suggested

This article describes an efficient method for solution-phase parallel synthesis of 2-quinoxalinol salen Schiff-base ligands. The novelty of this article is the synthesis of a new category of ligands using Schiff-base condensation of an aldehyde with a...

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N-Heterocyclic Carbene-Catalyzed [3+4] Cycloaddition and Kinetic Resolution of Azomethine Imines


09 Dec 2016

Suggestions for Improvement

The authors describe the syntheses of several optically pure [3+4] cycloaddition product from the reaction of racemic azomethine imines and enals using indanol-derived catalyst D having N-mesityl substituent.  This work pertains to the development of...

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A General Synthetic Route to Defined, Biologically Active Multivalent Arrays


09 Dec 2016

Good experimental, sub DIC for EDCI

The coupling reaction between a carboxylic acid and an alcohol to generate an ester needs a carbodiimide coupling agent. in the reference, the authors report the use of EDCI to prepare compound 1. I have used the same procedure in the synthesis of 1 though...

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High Turnover Number and Rapid, Room-Temperature Amination of Chloroarenes Using Saturated Carbene Ligands


09 Dec 2016

Reproducible Catalyst System

I need prepare a series of 2-amino-pyridines around 2003, and found this paper by SciFinder. 

I tested the reaction of 1-Boc-piperidine and 2-chloro-3-methyl- pyridine in 50mg scale using 5 mmol% catalysts.

The reactions were not completed in 3h at rt....

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Use of the Nonionic Superbase P(MeNCH 2 CH 2 ) 3 N in the Selective Monoalkylation of Active-Methylene Compounds


09 Dec 2016

Not reproducible. Experimental produced mixture

This paper by Verkade and co-workers describes a superbase P(MeNCH2CH2)3N mediated selective monoalkylation of active-methylene compounds. Although malonate alkylation has been known for many years, it is very difficult to obtain really good yields for...

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Mild Decarboxylative Activation of Malonic Acid Derivatives by 1,1′-Carbonyldiimidazole


09 Dec 2016

Wide versatility and good reproducibility

This work by Lafrance and co-work represents a very mild means to induce the decarboxylation of malonic acid derivatives with 1,1-carbonyldiimidazole (CDI). The reactive intermediate carbonyl imidazole moiety can be trapped with various nucleophiles in an...

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