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The Analytical Scientist / App Notes / 2016 / In-process control of ergoline psychedelics during chemical synthesis by HPTLC

In-process control of ergoline psychedelics during chemical synthesis by HPTLC

06/07/2016

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Introduction

TLC is a simple and convenient tool for monitoring classical organic syntheses. Standardized HPTLC may additionally provide reliable analytical endpoints and significantly improved separation. Structure confirmation can be achieved with HPTLC-MS hyphenation. In addition, HPTLC can be used as a technique complementary to existing HPLC methods for ensuring a product of high purity.

This method is suitable for identification of synthesis products. The CAMAG TLC-MS Interface 2 is used to directly elute target zones from the HPTLC plate into the Waters ACQUITY QDa® for mass detection. A second confirmation can be achieved by recording the UV spectra with the TLC scanner. A fast way for in-process and quality control during synthesis of ergoline psychedelics is shown below.

Synthesis of ergoline psychedelics

In a first step lysergic acid (LysS) is produced from ergotamine as starting material. Then the formation of different amides takes place, with LSD, LSZ, LSP, and LSM as finished products.

Figure 1: LysS is the starting material for the synthesis of LSD, LSZ, LSP, and LSM; different side chains are highlighted in red
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