MétaCan
Menu
Back to cohort
Record W2150048707 · doi:10.1002/047084289x.rn01600

5-Chloro-1-aza-5-stannabicyclo[3.3.3]undecane

2013· reference-entry· en· W2150048707 on OpenAlex

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.

affAt least one author lists a Canadian institution in the pinned OpenAlex snapshot.

Bibliographic record

VenueEncyclopedia of Reagents for Organic Synthesis · 2013
Typereference-entry
Languageen
FieldChemistry
TopicOrganometallic Compounds Synthesis and Characterization
Canadian institutionsUniversity of Waterloo
Fundersnot available
KeywordsUndecaneTransmetalationReagentChemistryYield (engineering)Redistribution (election)Intramolecular forceAlkylMedicinal chemistryOrganic chemistryCatalysisMaterials science

Abstract

fetched live from OpenAlex

(5-Chloro-1-aza-5-stannabicyclo[3.3.3]undecane) [93253-73-7] C9H18ClNSn (MW 294.41) InChI = 1S/C9H18N.ClH.Sn/c1-4-7-10(8-5-2)9-6-3;;/h1-9H2;1H;/q;;+1/p-1 InChIKey = BRPCJQRIZVVNKX-UHFFFAOYSA-M (precursor to organostannatranes that enable facile transfer of apical group due to intramolecular activation; selective alkyl transfer agent precursor) Alternate Name: 1-aza-5-chloro-5-stannabicyclo[3.3.3]undecane. Physical Data: mp 236–238 °C (EtOH),1 222–224 °C (MeOH).2 Solubility: soluble in Et2O, THF, EtOAc, CH2Cl2, and hexanes; slightly soluble in MeCN, MeOH, and i-PrOH; insoluble in H2O and aq. HCl. Form Supplied in: commercially available solid. Analysis of Reagent Purity: 13C and 119Sn NMR.3 Preparative Methods: initially prepared by transmetalation of N(CH2CH2CH2MgCl)34, 5 with SnCl4 in 12–15% yield. Subsequently, hydrozirconation of N(CH2CH–CH2)3 with Cp2ZrHCl followed by transmetalation with SnCl4 furnished 5-chloro-1-aza-5-stannabicyclo[3.3.3]undecane in 50% yield.2 Alternatively, 5-chloro-1-aza-5-stannabicyclo[3.3.3]undecane is prepared in 40% yield from N(CH2CH2CH2SnMe3)3 by thermal redistribution with Me2SnCl2.1, 5 N(CH2CH2CH2SnMe3)3 is synthesized by reacting N(CH2CH2CH2Cl)3 with Me3SnNa in liquid ammonia at −78 °C. Drawbacks to the preparation of chlorostannatrane by these routes are low yields, handling of volatile methyltin derivatives, harsh conditions, and/or expensive reagents. A scalable, two-step synthesis that remedies the former issues consists of the thermal redistribution of N(CH2CH2CH2SnBu3)3 with SnCl4 (eq 1). The tributylstannane N(CH2CH2CH2SnBu3)3 is accessible in 66% yield by the Pd/Al2O3-catalyzed hydrostannation of N(CH2CHCH2)3 with Bu3SnH, or alternatively, by the substitution of N(CH2CH2CH2Cl)3 with Bu3SnLi in 78% yield.6 (1) Purification: acid/base extraction6 or recrystallization from MeOH.2 Handling, Storage, and Precautions: toxic by ingestion and is a skin, eye, and respiratory tract irritant.7

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)0.002
Version: codex-gemma-dda1882f352aValidation status: machine_predicted_unvalidated
Candidate categoriesMeta-epidemiology (narrow), Research integrity, Insufficient payload (model declined to judge)
Consensus categoriesnone
DomainCandidate signal: none · Consensus signal: none
Study designCandidate signal: Not applicable · Consensus signal: none
GenreCandidate signal: Other · Consensus signal: Other
Teacher disagreement score0.604
Threshold uncertainty score1.000

Codex and Gemma teacher scores by category

CategoryCodexGemma
Metaresearch0.0000.002
Meta-epidemiology (narrow)0.0010.001
Meta-epidemiology (broad)0.0020.001
Bibliometrics0.0000.000
Science and technology studies0.0000.000
Scholarly communication0.0000.000
Open science0.0010.000
Research integrity0.0010.001
Insufficient payload (model declined to judge)0.0750.001

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 head0.015
GPT teacher head0.229
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