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Record W4391130339 · doi:10.1021/acs.cgd.3c01245

Exploring Polymorphism: Hydrochloride Salts of Pitolisant and Analogues

2024· article· en· W4391130339 on OpenAlexafffund
Jessica Patel, Zachary Leduc, Aaron Gabriel Nunez Avila, Joseph Glover, Kelin Wu, Yuxing Zhang, Jing Zhang, Xiaoting Zhai, Huize Jing, Alex M. Chen, Daniel Chartrand, Thierry Maris, Graeme M. Day, James D. Wuest

Bibliographic record

VenueCrystal Growth & Design · 2024
Typearticle
Languageen
FieldChemistry
TopicMolecular spectroscopy and chirality
Canadian institutionsUniversité de Montréal
FundersMitacsH2020 European Research CouncilCanada Research ChairsNatural Sciences and Engineering Research Council of CanadaEuropean CommissionUniversity of SouthamptonCanada Foundation for Innovation
KeywordsHydrochlorideChemistryPolymorphism (computer science)MetastabilityMonoclinic crystal systemCrystallographyCrystal structureOrganic chemistry

Abstract

fetched live from OpenAlex

Pitolisant hydrochloride is used to treat excessive daytime sleepiness in adults with narcolepsy. The drug is formulated as a crystalline solid, and a monoclinic P 2 1 form has been claimed in patents, but little additional information about the structure and polymorphism of the compound has been published. No new forms were obtained when we grew crystals from solution under various conditions. Re-examination of the crystals revealed a disordered and partially hydrated structure that resembles the one reported earlier but is not identical. Further insight was obtained by synthesizing analogues of pitolisant with its Cl substituent replaced by Me, F, and Br, followed by structural analysis of the hydrochloride salts by X-ray diffraction. Pitolisant hydrochloride and its three analogues showed very similar solid-state behavior, and each compound yielded new metastable forms when crystallized from melts. The lifetime of metastable form III of pitolisant hydrochloride could be extended significantly by adding small amounts of the fluoro analogue, but none of the metastable forms could be obtained as single crystals suitable for structural analysis. Computational predictions of the polymorphic landscapes of pitolisant hydrochloride and its analogues identified possible structures of the metastable forms. Dual experimental and computational approaches are already widely used in polymorphic screening, but our work shows the value of broadening these searches to include sets of structural analogues.

Fetched live from OpenAlex and de-inverted. Abstracts are not stored in this database: the inverted indexes are 8.6 GB of the frame’s 9.3 GB of text, and the host has 13 GB free.

How this classification was reachedexpand

Full frame distilled prediction

Teacher imitation

Not calibrated prevalence, not ground truth. Human validation pending. Learned from the 10,348 direct Codex labels and 10,348 direct Gemma labels. Candidate is the union of thresholded teacher heads; consensus is their intersection. These outputs are machine_predicted_unvalidated and are not human labels or direct frontier model labels.

metaresearch head score (Codex)0.000
metaresearch head score (Gemma)0.000
Version: codex-gemma-dda1882f352aValidation status: machine_predicted_unvalidated
Candidate categoriesnone
Consensus categoriesnone
DomainCandidate signal: none · Consensus signal: none
Study designCandidate signal: Bench or experimental · Consensus signal: Bench or experimental
GenreCandidate signal: Empirical · Consensus signal: Empirical
Teacher disagreement score0.029
Threshold uncertainty score0.733

Codex and Gemma teacher scores by category

CategoryCodexGemma
Metaresearch0.0000.000
Meta-epidemiology (narrow)0.0000.000
Meta-epidemiology (broad)0.0000.000
Bibliometrics0.0000.000
Science and technology studies0.0000.000
Scholarly communication0.0000.000
Open science0.0000.000
Research integrity0.0000.000
Insufficient payload (model declined to judge)0.0000.000

Machine scores (provisional)

The two teacher heads of the student model, read on this work. A score orders the frame for review; it never asserts a category, and the validation status ships verbatim with every row.

Baseline scores from an immature model (maturity gate not passed, 7 training rounds). Scores rank; they never assert a category.

Opus teacher head0.072
GPT teacher head0.251
Teacher spread0.179 · how far apart the two teachers sit on this one work
Validation statusscore_only:v0-immature-baseline · verbatim from the scoring run: score_only means the number may rank works, and no category label ships from it

Classification

machine, unvalidated

Machine predicted; a candidate call from one teacher head, not a consensus.

The models applied no category: nothing in the taxonomy fit this work.
Study designBench or experimental
Domainnot available
GenreEmpirical

How this classification was reached, model by model and score by score, is at the end of the page under "How this classification was reached".

Quick stats

Citations4
Published2024
Admission routes2
Has abstractyes

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