Issue 27, 2024

Preparation of sulfur–MOF composites and their application in the Willgerodt–Kindler reaction

Abstract

In this study, we demonstrate the successful synthesis of sulfur–MOF composites and their application in the Willgerodt–Kindler reaction. We showed that MIL-53(Al), CAU-10-H and MIL-101(Cr) encapsulate the sulfur without MOF decomposition by the melt-diffusion technique, whereas MIL-88A and MIL-101(Fe) were unable to form S@MOF composites. Various techniques, including XRD, SEM, EDS, and porometry, were used to characterize the synthesized S@MOF composites. The influence of MOF nature, temperature, reaction time and reagent ratio on the Willgerodt–Kindler reaction product formation was evaluated. The S@CAU-10-H composite led to the thiomorpholides from various arylaldehydes, acetophenones and propiophenones in 56–91% isolated yields. The reaction proceeds at near equimolar reactant concentrations. Product isolation is straightforward and does not require tedious chromatographic purification. The MOF was easily separated and reused in five runs, achieving a good performance without significant framework degradation. We postulate that the MOF has multiple roles, acting as a reaction medium, sulfur carrier, amine absorber and dehydration agent.

Graphical abstract: Preparation of sulfur–MOF composites and their application in the Willgerodt–Kindler reaction

Supplementary files

Article information

Article type
Paper
Submitted
21 Mar 2024
Accepted
14 Jun 2024
First published
14 Jun 2024

New J. Chem., 2024,48, 12444-12449

Preparation of sulfur–MOF composites and their application in the Willgerodt–Kindler reaction

A. V. Sokolov and E. A. Kvetkin, New J. Chem., 2024, 48, 12444 DOI: 10.1039/D4NJ01335B

To request permission to reproduce material from this article, please go to the Copyright Clearance Center request page.

If you are an author contributing to an RSC publication, you do not need to request permission provided correct acknowledgement is given.

If you are the author of this article, you do not need to request permission to reproduce figures and diagrams provided correct acknowledgement is given. If you want to reproduce the whole article in a third-party publication (excluding your thesis/dissertation for which permission is not required) please go to the Copyright Clearance Center request page.

Read more about how to correctly acknowledge RSC content.

Social activity

Spotlight

Advertisements