Search results for "yield"
showing 10 items of 1338 documents
Spectrophotometric determination of cystine by formation of an o-phthalaldehyde/N-acetyl-l-cysteine derivative
1989
Abstract Cystine reacts with o -phthalaldehyde (OPA) in the absence and presence of a thiol compound to yield different compounds. The use of N -acetyl- l -cysteine as thiol leads to the formation of two derivatives, likely simple and double isoindoles, where the disulfide bond remains unbroken. In contrast, mercaptoethanol gives rise to the reduction of the amino acid to form a cysteine derivative. Obtaining cystine isoindoles makes it possible to spectrophotometrically determine the amino acid after Chromatographic separation and is further evidence of the large stabilization effect produced by N -acetyl- l -cysteine in the formation of OPA-thiol derivatives.
Highly Enantioselective Protonation of the 3,4-Dihydro-2- methylnaphthalen-1(2H)-one Li-Enolate by TADDOLs
2000
A series of nine TADDOLs (=α,α,α′,α′-tetraaryl-1,3-dioxolane-4,5-dimethanols) 1a – 1i, have been tested as proton sources for the enantioselective protonation of the Li-enolate of 2-methyl-1-tetralone (=3,4-dihydro-2-methylnaphthalen-1(2H)-one). The enolate was generated directly from the ketone (with LiN(i-Pr)2 (LDA)/MeLi) or from the enol acetate (with 2 MeLi) or from the silyl enol ether (with MeLi) in CH2Cl2 or Et2O as the solvent (Scheme). The Li-enolate (associated with LiBr/LDA, or LiBr alone) was combined with 1.5 – 3.0 equiv. of the TADDOL at −78° by addition of the latter or by inverse addition. 2-Methyl-1-tetralone of (S)-configuration is formed (≤80% yield) with up to 99.5% sele…
Radioactively labelled epoxides part II. (1) tritium labelled cyclohexene oxide, transstilbene oxide and phenanthrene 9,10-oxide
1980
Tritium labelled cyclohexene oxide, trans-stilbene oxide and phenanthrene 9,10-oxide were prepared with specific activities of 0.7 - 1.1 mCi per mmole starting with monoor diketo compounds. Tritium was introduced by reducing the ketone precursors with tritiated complex metal hydrides. The resulting alcohols were transformed to the epoxides by methods described for the unlabelled compounds. The syntheses require only two or three steps and yield cyclohexene oxide, trans-stilbene oxide and phenanthrene 9,10-oxide, important substrates for the study of epoxide hydratase and glutathione S-transferases in high radiochemical purity.
Stereoselective synthesis of syn-α-methyl-β-hydroxy esters
2000
Abstract Boron enolates of an ethyl ketone structurally related to erythrulose react with achiral aldehydes in a highly stereoselective fashion to yield 1,2- syn /1,3- syn stereoisomers. Oxidative cleavage of the aldol adducts yields enantiopure O -formylated syn -α-methyl-β-hydroxy esters, easily cleaved to the corresponding hydroxyl-free compounds. The aforementioned ketone behaves therefore as a chiral propionate enolate equivalent.
Semiconductor Nanocrystals with Multifunctional Polymer Ligands
2002
In this letter, we describe the preparation of a versatile polymer ligand, which can be attached to CdSe/ZnS semiconductor nanocrystals via a phase transfer reaction. The ligand is based on a chain of reactive esters, which can, in principle, be substituted by any compound containing amino-functionalities. The polymer/nanocrystal complexes are characterized in terms of structure and photostability.
Maximizing the emissive properties of CH3NH3PbBr3 perovskite nanoparticles
2015
Highly luminescent and photostable CH3NH3PbBr3 nanoparticles have been prepared by fine-tuning the molar ratio between CH3NH3Br, PbBr2, a medium-size alkyl-chain ammonium salt, and 1-octadecene. The nanoparticles exhibit an excellent photoluminescence quantum yield (ca. 83%) and average recombination lifetime (ca. 600 ns) in toluene dispersion.
Design, Synthesis, and Use of Y-Shaped ATRP/NMP Surface Tethered Initiator.
2015
Heterogeneous polymer brushes on surfaces can be easily formed from a binary initiator on a silicon oxide substrate where two different types of polymers can be grown side-by-side. Herein, we designed a new Y-shaped binary initiator using straightforward chemistry for “grafting from” polymer brushes. This initiator synthesis takes advantage of the Passerini reaction, a multicomponent reaction combining two initiator sites and one surface linking site. This Y-shaped binary initiator can be synthesized in three steps with a higher yield than other similar initiators reported in the literature, and can be performed on a multigram scale. We were able to attach the initiator to a silicon oxide s…
Controlled Synthesis of Linear Polymers with Highly Branched Side Chains by “Hypergrafting”: Poly(4-hydroxy styrene)-graft-hyperbranched Polyglycerol
2012
Linear polymers with hyperbranched side chains are unusual macromolecular structures due to their high number of functional groups in the side chains as well as their potential cylindrical conformation in bulk or solution. In a three-step synthesis combining anionic and oxy-anionic polymerization, hyperbranched polyglycerol was “hypergrafted” from linear poly(4-hydroxy styrene) macroinitiators to yield poly(4-hydroxy styrene)-graft-hyperbranched polyglycerol. Successful grafting with control over molecular weight (10–31 kg·mol–1) and low PDIs (<1.4) was shown by various characterization techniques. All polymers have a high side chain density, due to rapid transfer of the initiating function…
Asymmetric One-Pot Synthesis of (3R,3aS,6aR)-Hexahydrofuro[2,3-b]furan-3-ol: A Key Component of Current HIV Protease Inhibitors
2017
A concise and efficient synthesis of (3R,3aS,6aR)-hexahydrofuro[2,3-b]furan-3-ol, a key building block for several clinical and experimental HIV protease inhibitors including the highly important drug darunavir, was achieved via a one-pot procedure using furan and Cbz-protected glycol aldehyde as starting materials. A [2+2]-photocycloaddition between both reactants which can be prepared from wood-based starting materials according to the principles of xylochemistry, followed by hydrogenation and lipase-catalyzed kinetic resolution afforded the target compound in high yield and up to 99% ee.
Diastereoselective synthesis of fluorinated, seven-membered beta-amino acid derivatives via ring-closing metathesis.
2003
[reaction: see text] Cis and trans seven-membered gamma,gamma-difluorinated beta-amino acid derivatives (III) have been prepared with a sequence that starts with imidoyl halides (I), which are condensed with suitable ester enolates to give intermediates (II). These, in turn, can be cyclized by means of a ring-closing olefin metathesis reaction and the product stereoselectively reduced to yield compounds (III) in good overall yields.