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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...

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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...

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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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Photoinduced, Copper-Catalyzed Alkylation of Amides with Unactivated Secondary Alkyl Halides at Room Temperature


01 Nov 2016

Coupling N-alkylation of Amides with Secondary Alkyl Halides

Yapin Wang

Emaill: ywang2@lsuhsc.edu

1) Reaction of Standard Condition
Using photo-induced (hn 254), copper- catalyzed (10% CuI), two ratio base(LiOt-Bu), CH3CN/DMF as solvents and
stirring for 24 hrs at room temperature, Amides react with inactivated...

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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...

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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...

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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...

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(R)- and (S)-4-TIPS-3-butyn-2-ol. Useful Precursors of Chiral Allenylzinc and Indium Reagents


01 Nov 2016

Synthesis of the optically active TIPS-functionalized acetylenic alcohols

A detailed route for the synthesis of the "S" enantiomer of 4-TIPS-3-butyn-2-ol in 90% enantiomeric purity by reduction of the ynone precursor by the Noyori catalytic system was reported by Marshall et al. The ease of catalyst preparation, operational...

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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...

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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...

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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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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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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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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...

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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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Alkyl-Substituted Polyaminohydroxamic Acids:  A Novel Class of Targeted Histone Deacetylase Inhibitors


01 Nov 2016

Reproducible synthesis of compound 20

Synthesized (20) using the similar (not exactly same) procedure (Scheme 2) as was written in the paper.

1,4-Diaminobutane was firstly protected by mesitly chloride in DCM (overnight under reflux condition). The protected intermediate was then...

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Synthesis of Ethyl (1S,2R,3S,4S,5S)-2,3-O-(Isopropylidene)-4-Hydroxy-Bicyclo[3.1.0]Hexane-Carboxylate from L-Ribose: A Versatile Chiral Synthon for Preparation of Adenosine and P2 Receptor Ligands


01 Nov 2016

Convenient and reproducible synthetic methodology for North configured ribose containing mono phosphate

The article is about versatile synthetic strategy for preparing enantiomerically pure (N)-methanocarba ring containing monophosphates as a potent agonist for P2 receptors. 

I have successfully reproduced the synthesis of compound (2, MRS2339) from...

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Preparation and characterisation of fluorescent chitosans using 9-anthraldehyde as fluorophore


01 Nov 2016

Quality paper, good reproducibility


The procedure was adapted for the covalent attachment of an organometallic complex to chitosan backbone for use in a glucose oxidase bioanode. The procedure was done in both acidic (as in paper) and basic conditions (for comparison) for the following...

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