Date of Award

12-2025

Degree Type

Dissertation

Degree Name

Doctor of Philosophy (PhD)

School

Mathematics and Natural Sciences

Committee Chair

Dr. Douglas Masterson

Committee Chair School

Mathematics and Natural Sciences

Committee Member 2

Dr. Julie Pigza

Committee Member 2 School

Mathematics and Natural Sciences

Committee Member 3

Dr. Karl Wallace

Committee Member 3 School

Mathematics and Natural Sciences

Committee Member 4

Dr. Wujian Miao

Committee Member 4 School

Mathematics and Natural Sciences

Committee Member 5

Dr. Robert J Hondal

Abstract

The “Malonate Template” provides access to various amino acids, all from a common intermediate. Herein, demonstrates the use of the malonate template to establish a synthetic route to both 2-thiohistidine and 2-thio-3-N-methyl-histidine from a benzyl methyl malonate derived intermediate. Furthermore, efforts exploiting the applicability of the malonate template for the of both 2-thiohistidine and 2-thio-3-N-methyl-histidine as a suitable alternative to methods previously described by Erdelmeier are described.

The method presented incorporates modifications to the biomimetic pathway described by Erdelmeier for the synthesis of 2-thiohisidine. By exploiting the biomimetic formation of 2-thiohisitidne’s mechanism via mass spectrometry, we demonstrated that 2-thiohsitidine is a by-product of a β-elimination of DHA from the cysteine adduct proposed by Erdelmeier. Accordingly, we were able to incorporate the pathway into our malonate template for a more efficient and versatile synthesis of both 2-thiohsitidne and 2-thio-3-N-methyl-histidine.

Furthermore, with many enantioenriched novel amino acids synthesized previously from the malonate template, we sought to develop a method for rapidly assessing the optical purity of the malonate derived novel amino acids using a deuterium labeled probe for quantifying optical purity directly from 1H-NMR. Our results or consistent with those demonstrated by HPLC and carbon-13 labeling from assaying PLE and six iso-enzymes.

ORCID ID

0000-0002-0576-4005

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