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1.
Bioorg Med Chem Lett ; 25(19): 4104-8, 2015 Oct 01.
Article in English | MEDLINE | ID: mdl-26321360

ABSTRACT

A high throughput screen allowed the identification of N-hydroxyimide inhibitors of ERCC1-XPF endonuclease activity with micromolar potency, but they showed undesirable selectivity profiles against FEN-1. A scaffold hop to a hydroxypyrimidinone template gave compounds with similar potency but allowed selectivity to be switched in favour of ERCC1-XPF over FEN-1. Further exploration of the structure-activity relationships around this chemotype gave sub-micromolar inhibitors with >10-fold selectivity for ERCC1-XPF over FEN-1.


Subject(s)
DNA-Binding Proteins/antagonists & inhibitors , Endonucleases/antagonists & inhibitors , Imides/pharmacology , Pyrimidinones/pharmacology , DNA Repair , Dose-Response Relationship, Drug , Flap Endonucleases/antagonists & inhibitors , Hep G2 Cells , Humans , Imides/chemistry , Molecular Structure , Pyrimidinones/chemistry , Structure-Activity Relationship
2.
Bioorg Med Chem Lett ; 25(19): 4097-103, 2015 Oct 01.
Article in English | MEDLINE | ID: mdl-26318993

ABSTRACT

Catechol-based inhibitors of ERCC1-XPF endonuclease activity were identified from a high-throughput screen. Exploration of the structure-activity relationships within this series yielded compound 13, which displayed an ERCC1-XPF IC50 of 0.6 µM, high selectivity against FEN-1 and DNase I and activity in nucleotide excision repair, cisplatin enhancement and γH2AX assays in A375 melanoma cells. Screening of fragments as potential alternatives to the catechol group revealed that 3-hydroxypyridones are able to inhibit ERCC1-XPF with high ligand efficiency, and elaboration of the hit gave compounds 36 and 37 which showed promising ERCC1-XPF IC50 values of <10 µM.


Subject(s)
Catechols/pharmacology , DNA Repair/drug effects , DNA-Binding Proteins/antagonists & inhibitors , Endonucleases/antagonists & inhibitors , Pyridones/pharmacology , Catechols/chemistry , Cell Line, Tumor , Deoxyribonuclease I/antagonists & inhibitors , Deoxyribonuclease I/metabolism , Dose-Response Relationship, Drug , Flap Endonucleases/antagonists & inhibitors , Humans , Molecular Structure , Pyridones/chemistry , Structure-Activity Relationship
3.
Science ; 377(6612): 1323-1328, 2022 09 16.
Article in English | MEDLINE | ID: mdl-36108027

ABSTRACT

The generation of carbon radicals by halogen-atom and group transfer reactions is generally achieved using tin and silicon reagents that maximize the interplay of enthalpic (thermodynamic) and polar (kinetic) effects. In this work, we demonstrate a distinct reactivity mode enabled by quantum mechanical tunneling that uses the cyclohexadiene derivative γ-terpinene as the abstractor under mild photochemical conditions. This protocol activates alkyl and aryl halides as well as several alcohol and thiol derivatives. Experimental and computational studies unveiled a noncanonical pathway whereby a cyclohexadienyl radical undergoes concerted aromatization and halogen-atom or group abstraction through the reactivity of an effective H atom. This activation mechanism is seemingly thermodynamically and kinetically unfavorable but is rendered feasible through quantum tunneling.

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