Related Experiment Video
Updated: Apr 16, 2026

Light-driven Enzymatic Decarboxylation
Published on: May 22, 2016
Method development and validation of arene substituted regioisomers in a pharmaceutical candidate by high temperature
John J Salisbury1, Nga M Do2, John A Ragan2
1Analytical Research and Development, Pfizer Worldwide Research and Development, Eastern Point Road, Groton, CT 06340, USA.
Abstract:
This paper describes the development and validation of a high temperature gas chromatography flame ionization detection (HTGC-FID) method for the purity evaluation of arene substituted regioisomers in a key starting material of a pharmaceutical candidate in Phase 3 studies. The chromatographic conditions of the method employ a (5%-phenyl)-methylpolysiloxane packed column (30m×0.25mm) at a constant flow of 1.0mLmin(-1) with a gradient temperature program from 150°C to 400°C with injector and detector temperatures of 300°C and 340°C, respectively. The calibration curve for the desired product (r=0.9999) was assessed for five points in the range from approximately 1.0μgmL(-1) to 40μgmL(-1). The precision (% RSD) of the method was calculated for six replicate injections and found to be 0.81%. The limits of detection and quantitation were determined to be 0.06 and 0.20μgmL(-1), respectively.
More Related Videos
10:33Development of Inhibitors of Protein-protein Interactions through REPLACE: Application to the Design and Development Non-ATP Competitive CDK Inhibitors
Published on: October 26, 2015
10:14Synthesis and Purification of Iodoaziridines Involving Quantitative Selection of the Optimal Stationary Phase for Chromatography
Published on: May 16, 2014
Related Concept Videos
Regioselectivity and Stereochemistry of Hydroboration
Hydroboration proceeds in a concerted fashion with the attack of borane on the π bond, giving a cyclic four-centered transition state. The –BH2 group is bonded to the less substituted carbon and –H to the more substituted carbon. The concerted nature requires the simultaneous addition of –H and –BH2 across the same face of the alkene giving syn...
Stability of Substituted Cyclohexanes
The two chair conformations of cyclohexanes undergo rapid interconversion at room temperature. Both forms have identical energies and stabilities, each comprising equal amounts of the equilibrium mixture. Replacing a hydrogen atom with a functional group makes the two conformations energetically non-equivalent.
For example, in...
Regioselectivity of Electrophilic Additions to Alkenes: Markovnikov's Rule
The hydrohalogenation of an unsymmetrical alkene can yield two haloalkane products, depending on which vinylic carbon takes up the halogen. However, one product usually predominates, where hydrogen adds to the vinylic carbon bearing the...
Reduction of Alkenes: Asymmetric Catalytic Hydrogenation
The metal catalyst used can be either heterogeneous or homogeneous. When hydrogenation of an alkene generates a chiral center, a pair of enantiomeric products is expected to form. However, an enantiomeric excess of one of the products can be facilitated using an enantioselective reaction or an...
Preparation of 1° Amines: Hofmann and Curtius Rearrangement Overview
Preparation of 1° Amines: Hofmann and Curtius Rearrangement Mechanism