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Record W4367843587 · doi:10.26434/chemrxiv-2023-0xbh5

Active, selective, and stable single-component precatalysts for asymmetric allylic alkylation

2023· preprint· en· W4367843587 on OpenAlexafffund
Jingjun Huang, Thomas Keenan, F. Richard, Jingru Lu, Sarah E. Jenny, Alexandre Jean, Stellios Arseniyadis, David C. Leitch

Bibliographic record

VenueChemRxiv · 2023
Typepreprint
Languageen
FieldChemistry
TopicAsymmetric Synthesis and Catalysis
Canadian institutionsUniversity of Victoria
FundersNatural Sciences and Engineering Research Council of CanadaServierBritish Columbia Knowledge Development FundQueen Mary University of LondonUniversity of Victoria
KeywordsTsuji–Trost reactionChemistryEnantioselective synthesisCombinatorial chemistryCatalysisAllylic rearrangementPalladiumAlkylationSelectivityLigand (biochemistry)Chiral ligandStereoselectivityOrganic chemistry

Abstract

fetched live from OpenAlex

The stereoselective construction of new carbon-element bonds is a crucial aspect of organic synthesis. Among the many strategies developed to date, palladium-catalysed asymmetric allylic alkylation is commonly used to access chiral molecules in natural product and active pharmaceutical ingredient synthesis. The use of modular Trost-type ligands and phosphinooxazoline (PHOX) ligands results in generally high stereoselectivity for a wide range of transformations. However, these reactions nearly always require relatively high catalyst loadings (5-10 mol%), reaction-specific catalyst preactivation protocols, and excess chiral ligand to ensure high yield and selectivity. Here we report the isolation and catalytic evaluation of a series of chiral palladium(0) single-component precatalysts that are active for a variety of asymmetric allylic alkylation reactions. The four Trost-type precatalysts in this work are the first characterized examples of stable, isolable Pd complexes with the diphosphines coordinated in the desired κ2-P,P fashion. All of the palladium(0) complexes are stable for >12 months when stored under nitrogen, and can be handled as solids and even in solution under air for hours without decomposition. A catalytic evaluation of these single-component precatalysts across 9 distinct asymmetric allylic alkylation reactions reveals excellent performance in terms of reactivity, selectivity, practicality, and minimizing palladium and chiral ligand loading. This enables both small-scale multivariate screening studies and preparative scale synthesis of key chiral building blocks, exemplified with the unprecedented enantioselective allylation of hydantoins. The optimized reaction achieves high yield and enantioselectivity with only 0.2 mol% of catalyst (turnover number of 465). These precatalysts will enable development of more efficient and robust asymmetric allylic alkylation reactions toward complex target molecules.

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)0.001
Version: codex-gemma-dda1882f352aValidation status: machine_predicted_unvalidated
Candidate categoriesMeta-epidemiology (narrow)
Consensus categoriesnone
DomainCandidate signal: none · Consensus signal: none
Study designCandidate signal: Bench or experimental · Consensus signal: none
GenreCandidate signal: Empirical · Consensus signal: Empirical
Teacher disagreement score0.714
Threshold uncertainty score1.000

Codex and Gemma teacher scores by category

CategoryCodexGemma
Metaresearch0.0000.001
Meta-epidemiology (narrow)0.0010.001
Meta-epidemiology (broad)0.0010.000
Bibliometrics0.0010.001
Science and technology studies0.0000.000
Scholarly communication0.0000.000
Open science0.0000.001
Research integrity0.0010.000
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 head0.041
GPT teacher head0.256
Teacher spread0.215 · 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.

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

Citations1
Published2023
Admission routes2
Has abstractyes

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