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Record W2009676237 · doi:10.1139/v03-211

Concerning the mechanism of the Friedländer quinoline synthesis

2004· article· en· W2009676237 on OpenAlex
Joseph M. Muchowski, Michael L. Maddox

Why this work is in the frame

A frame that forgets how it found something cannot be audited. These are the routes that admitted this work.

venuePublished in a venue whose home country is Canada.
no affNo Canadian affiliation: this work is invisible to an affiliation-only frame.
No Canadian affiliation. An affiliation-only frame, the usual design, would never have seen this work. It is one of the works that make the case for inverting the frame.

Bibliographic record

VenueCanadian Journal of Chemistry · 2004
Typearticle
Languageen
FieldChemistry
TopicAnalytical Chemistry and Chromatography
Canadian institutionsnot available
Fundersnot available
KeywordsChemistryAldehydeQuinolineKetoneAdductAldol reactionTrifluoromethanesulfonateAldol condensationSchiff baseMedicinal chemistryTolueneCatalysisDerivative (finance)Reactivity (psychology)Organic chemistryStereochemistry

Abstract

fetched live from OpenAlex

Detailed experiments regarding the mechanism of the Friedländer synthesis of quinolines from o-aminobenzaldehydes and simple aldehydes or ketones are described. Under the basic or acidic conditions commonly used in this reaction, it is concluded that the first step involves a slow intermolecular aldol condensation of the aldehyde or ketone with the o-aminobenzaldehyde. The aldol adduct 5 generated in this manner then undergoes very rapid cyclization to 4, which subsequently loses water to produce the quinoline derivative 8. Both 5 and 4 are too short lived to be detectable (TLC), even when deliberately generated by other means. It is also shown that E-enones corresponding to 6, i.e., the aldol dehydration product, are converted into quinolines (e.g., 21a and 21b from 17a and 17b) under basic or acidic conditions. Such enones are not detected as intermediates in the base-induced Friedländer synthesis, even though certain congeners (17b) would be easily observable. Under acidic conditions these enones are too short lived to be detectable. Schiff bases derived from 2-aminobenzaldehyde (18a) and aldehydes or ketones can be generated under special conditions, but they show reactivity patterns different from those seen in the usual Friedländer condensations. Thus, the ytterbium-triflate-catalyzed reaction of aldehydes with 18a at room temperature in toluene generates the E-Schiff bases (33, R 1 = H), from which isomeric mixtures of tetrahydroquinoline derivatives 26 are formed exclusively. At higher temperatures, the E-Schiff bases 33 are isomerized to the Z-Schiff bases 34, from which the 3-substituted quinoline derivatives 24 are formed as the major products under appropriate conditions. Also, the ytterbium-triflate-catalyzed reaction of 18a with the pyrrolidine enamines of the methyl-n-alkylketones 38a,b produces mixtures in which the 2-monosubstituted kinetic products 37b,d predominate over the 2,3-disubstituted thermodynamic products 21c,e by a factor of 4:1 to 5:1. These results are opposite to those observed under the usual basic or acidic Friedländer reactions with methyl-n-alkylketones, where the thermodynamic products are usually strongly favored. The unusual kinetic:thermodynamic product ratios observed with 38a,b are ascribed to the generation and rapid cyclization of mixtures of the Schiff bases 35 and 36, in which the kinetic isomer 35 is highly predominant. Key words: mechanism, Friedländer synthesis, quinolines, intramolecular aldol reactions, Schiff bases, tetrahydroquinolines, high kinetic:thermodynamic product ratios.

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.

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 categoriesInsufficient payload (model declined to judge)
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 score0.037
Threshold uncertainty score0.999

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 science0.0010.000
Research integrity0.0000.001
Insufficient payload (model declined to judge)0.0020.000

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 head0.011
GPT teacher head0.192
Teacher spread0.181 · 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