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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...

(2)

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...

(2)

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...

(1)

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...

(2)

Enzymatic Synthesis of 7-Deoxy-N-acetylneuraminic Acid and 7-O-Methyl-N-acetylneuraminic Acid


09 Dec 2016

Modifications implemented to improve yields

I used the published synthethic methods for both deoxy and methoxy derivatives with some modifications and obtained a lot higher yields.

Deoxy: 2 eq of 1,1′-Thiocarbonyldiimidazole is enough (paper is 2.5 eq) and I used 1,2-dichloroethane instead of CH2Cl2...

(0)

Efficient, one-pot syntheses of biologically active α-linked glycolipids


09 Dec 2016

Adjustments needed to increase efficiency of methodology

The methodology described in this article is very valuable for scientists working with glycosphingolipids. It provided a one-pot syntheses of alpha-linked glycolipids with the possibility of using substrates with unsaturations in the fatty acid side...

(1)

Total Synthesis and Biological Evaluation of Glycolipids Plakosides A, B and Their Analogs


09 Dec 2016

Easy to follow procedures; yields not reproducible

In one of my Ph.D. projects where I was working on the total syntheses of glycosphingolipids, I followed this reference to prepare some of the intermediates. This is a very important publication in the glycolipid field since it is among the few papers that...

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Benzobisthiazole-Based Donor–Acceptor Copolymer Semiconductors for Photovoltaic Cells and Highly Stable Field-Effect Transistors


09 Dec 2016

Good synthesis; product easy to isolate

Synthesized 2,6-Bis(3-dodecylthiophen-2-yl)benzobisthiazole following the procedure.

(1) The reaction was reproduced with higher yields (>25%).

(2) Added the 2-carboxylaldehydethiophene derviative by portions, used longer reaction time (24hs) and...

(0)

CHLOROSULFONATION OF SOME POLYNUCLEAR HETEROCYCLIC COMPOUNDS


09 Dec 2016

Lacking complete isolation/purification procedures

This article reported the synthesis of different sulfonyl chloride of polynuclear heterocyclic compounds which are very important intermediates to form different derivatives like sulfonates. Unfortunately, this paper is lacking a complete isolation and...

(1)

Butane 2,3-Bisacetal Protection of Vicinal Diequatorial Diols


09 Dec 2016

Clear, Detailed Paper

After searching for an alternate protecting group for the protection of cis-dihydrocatechols, it was found that the butane-bisacetals were more resilient to hydrolysis. This is crucial when protecting group stabiity is required for acetals that are exposed to...

(2)

A Practical Synthesis of C2-Symmetric Chiral Binaphthyl Ketone Catalyst


09 Dec 2016

Several Recommendations for Improved Synthesis

Summary:

A practical synthesis of 11-membered C2-symmetric binaphthyl ketone (R)-1, a catalyst for asymmetric epoxidation, was developed. This manuscript describes the single example of chiral resolution of (±)-1,1’-Binaphthyl-2,2’-dicarboxylic acid [(±)-6...

(1)

Practical Synthesis of Unsymmetrical Ureas from Isopropenyl Carbamates


09 Dec 2016

Mild, High Yielding Method

Ureas are very widely used synthetic targets in pharmaceutical industry especially as kinase inhibitors. Using this methodology we have synthesized thousands of unsymmetrical ureas as kinase inhibitors. This method is a very mild, high yielding and can work...

(0)

Hydroboration. 97. Synthesis of New Exceptional Chloroborane−Lewis Base Adducts for Hydroboration. Dioxane−Monochloroborane as a Superior Reagent for the Selective Hydroboration of Terminal Alkenes†


09 Dec 2016

Equivalency of reagents key for successful synthesis

Review: Synthesized the same compound of Dioxane-Monochloroborane by the reaction of Sodium Borohydride with Dioxane-borontrichloride (experimental section, Page 5364). I found the equivalency of the reagents is very important for this reaction. The reaction...

(1)

Construction of the Bicyclo[3.1.0]hexane Template of a Conformationally Locked Carbocyclic Adenosine via an Olefin Keto-Carbene Cycloaddition


09 Dec 2016

Experimental Yields Lower than Literature

Victor E. Marquez et. al. first introduced the concept of locked conformations, 2'-exo (North) and 3'-exo (South), of ribose ring in nucleosides. In this article the synthetic methodology and successful synthesis of receamic and conformationally locked South...

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Enantiomers of 1-ethyl-7-[3-[(ethylamino)methyl]-1-pyrrolidinyl]-6,8-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid: preparation and biological activity


09 Dec 2016

Procedure Adapted for Better Synthesis

Wanting to avoid a chromatographic separation of the Me esters as well as the greater expense of dimethyl itaconate, the reaction of alpha methyl benzylamine and itaconic acid was performed in xylene.  The reaction was performed by adding the amine at 110 to...

(0)

Catalytic Isomerization of Cyanoolefins Involved in the Adiponitrile Process. C−CN Bond Cleavage and Structure of the Nickel π-Allyl Cyanide Complex Ni(η3-1-Me-C3H4)(CN)(dppb)


09 Dec 2016

Helpful experimental; Some discrepancies observed in NMR

The article reports the catalytic isomerization of the branched cyanoolefin 2-methyl-3-butenenitrile (2M3BN) to the linear isomer 3-pentenenitrile (3PN) using nickel-phosphine complexes.

The authors report that the optimal catalytic experiment was carried...

(0)

Isolation and reactions of .alpha.-lithio N,N-dimethylacetamide


09 Dec 2016

Reproducible Experimental

Summary: The paper discusses the synthesis, reactivity and stability of α-lithio N,N dimethylacetamide.

The paper described carefully the use of various solvents (pentane, THF) and their impact on the formation of the desired product.

It also described...

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