Effect of OH and F Substitution in Benzoic Acid Coformers on the Solubility and Permeability of Fluorinated Drug Roflumilast

Roflumilast (RML), a difluoromethyl and dichlorophenyl group-containing drug, is a selective phosphodiesterase-4 inhibitor (PDE-4). It is prescribed to mitigate the risk of exacerbations in patients with severe chronic obstructive pulmonary disease and to address plaque psoriasis. The presence of the F atom in drugs and intermolecular interactions and weak hydrogen bonds of fluorine are a contemporary theme in crystal engineering of pharmaceutical cocrystals. The aim of this study is to examine the effect of H ↔ F ↔ OH exchange in coformer molecules and their effect on hydrogen bonding and crystal packing. Three cocrystals of RML were successfully crystallized with 4-hydroxybenzoic acid (4HBA), 4-fluorobenzoic acid (4FBA, H ↔ F), and 3-fluoro-4-hydroxybenzoic acid (3F-4HBA, H ↔ F and F ↔ OH). Their X-ray crystal structures were analyzed for hydrogen bonding synthons and weak intermolecular interactions, notably involving the less common F atom. The presence of an amide tape supramolecular synthon of the N–H···O hydrogen bond along with an auxiliary Cl···O interaction is observed between RML molecules. The crystal structures of RML-4HBA and RML-3F-4HBA contain a Cl···O–(H) halogen bond, while in RML-4FBA, it is replaced by a Cl···F–(C) interaction, indicating OH ↔ F mimicry in cocrystal design. The solubility and dissolution rate of RML were investigated in a physiological environment to show that the cocrystal form exhibited an improved solubility and dissolution rate compared to pure RML. The fluoro coformers enhance drug bioavailability and membrane permeation.

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Publication Details

Journal
Crystal Growth & Design
Published
2025-04-19
DOI
https://doi.org/10.1021/acs.cgd.5c00191
Citations
1
Primary Topic
Fluorine in Organic Chemistry
Type
article
Field-Weighted Citation Impact
0.79

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article

Effect of OH and F Substitution in Benzoic Acid Coformers on the Solubility and Permeability of Fluorinated Drug Roflumilast

Ashwini Nangia, Shruti Sangwan, Abhijit Garai
1 citations
Crystal Growth & Design
Fluorine in Organic Chemistry
0.79
article

Effect of OH and F Substitution in Benzoic Acid Coformers on the Solubility and Permeability of Fluorinated Drug Roflumilast

Ashwini Nangia, Shruti Sangwan, Abhijit Garai
article en
1 citations

Abstract

Roflumilast (RML), a difluoromethyl and dichlorophenyl group-containing drug, is a selective phosphodiesterase-4 inhibitor (PDE-4). It is prescribed to mitigate the risk of exacerbations in patients with severe chronic obstructive pulmonary disease and to address plaque psoriasis. The presence of the F atom in drugs and intermolecular interactions and weak hydrogen bonds of fluorine are a contemporary theme in crystal engineering of pharmaceutical cocrystals. The aim of this study is to examine the effect of H ↔ F ↔ OH exchange in coformer molecules and their effect on hydrogen bonding and crystal packing. Three cocrystals of RML were successfully crystallized with 4-hydroxybenzoic acid (4HBA), 4-fluorobenzoic acid (4FBA, H ↔ F), and 3-fluoro-4-hydroxybenzoic acid (3F-4HBA, H ↔ F and F ↔ OH). Their X-ray crystal structures were analyzed for hydrogen bonding synthons and weak intermolecular interactions, notably involving the less common F atom. The presence of an amide tape supramolecular synthon of the N–H···O hydrogen bond along with an auxiliary Cl···O interaction is observed between RML molecules. The crystal structures of RML-4HBA and RML-3F-4HBA contain a Cl···O–(H) halogen bond, while in RML-4FBA, it is replaced by a Cl···F–(C) interaction, indicating OH ↔ F mimicry in cocrystal design. The solubility and dissolution rate of RML were investigated in a physiological environment to show that the cocrystal form exhibited an improved solubility and dissolution rate compared to pure RML. The fluoro coformers enhance drug bioavailability and membrane permeation.

Crystal Growth & DesignVol. 25(9)
University of Hyderabad (IN), Universidad Politécnica de El Salvador (SV), Advanced Engineering (Czechia) (CZ)
Department of Science and Technology, Ministry of Science and Technology, India, University Grants Commission, Ministry of Education, India, University of Hyderabad, Science and Engineering Research Board
Clean water and sanitation
Openalex Percentile: Top 29%
Fluorine in Organic Chemistry
0.79
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