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Buchwald–Hartwig amination, record ord-15613520ef9b4d099659a0a3ac545228

One recorded run of this reaction. Below is what the source recorded, and nothing added to it.

verified record43% yield recordedNot balanced as writtenFrom experimental reaction archive

Reactants and products as the record gives them. Reagents, catalysts and solvents are listed below rather than drawn.

Open this record in the Reaction LabThe atom map, the animation and the records that run the same transformation.

What was in the flask

RoleSpeciesFormulaYield
Reactant4-BromopyridineC₅H₄BrN
Reactant4-HydroxypyrrolidineC₄H₉NO
Reagentlithium bis(trimethylsilyl)azanideC₆H₁₈LiNSi₂
Catalyst2-(Dicyclohexylphosphino)-2'-(dimethylamino)biphenylC₂₆H₃₆NP
CatalystBis(dibenzylideneacetone)palladiumC₅₁H₄₂O₃Pd₂
SolventTetrahydrofuranC₄H₈O
Product1-(Pyridin-4-yl)pyrrolidin-3-olC₉H₁₂N₂O43.01%

The equation does not balance as written. That is usual for an experimental record: the source listed what it put in and what it measured, not a stoichiometric equation.

Conditions

Temperature
65 °C

Only the dimensions the source stated are listed. Anything absent here was not recorded, and it is not inferred from what the class usually needs.

Yield

  • 43% of 1-(Pyridin-4-yl)pyrrolidin-3-ol.

Procedure

Copied from the source record, unedited

In a 50 ml round bottomed flask THF (1 mL) was added to a mixture of 4-bromopyridine (1 g, 6.33 mmol), pyrrolidin-3-ol (0.662 g, 7.60 mmol),2-(dimethylamino)-2'-(dicyclohexylphosphino)biphenyl (0.249 g, 0.63 mmol) and Pd2(dba)3 (0.580 g, 0.63 mmol). To the slurry lithium bis(trimethylsilyl)amide (13.92 mL, 13.92 mmol) was added dropwise at 0 °C and the solution was refluxed at 65 °C overnight for 20 hrs. The reaction mixture was passed through celite, concentrated and column purified (0-20%MeOH/DCM) to obtain 0.447 mg of product.

The source

This record comes from experimental reaction archive (ord-15613520ef9b4d099659a0a3ac545228). Open the source and check it against what is on this page.

  • experimental reaction archive record ord-15613520ef9b4d099659a0a3ac545228 from dataset "750 AstraZeneca ELN dataset" (url: https://chemrxiv.org/engage/chemrxiv/article-details/60c9e3f37792a23bfdb2d471). No atom mapping is provided by the source.

    experimental record · quality medium · source

experimental reaction record.

How to read this record

This is one experiment, not a rule. It says that on one occasion these species were combined under these conditions and this came out. It does not say the reaction will give the same result on your substrate, and nothing on the page has been generalised into a claim that it would.

The pathway is a separate question, kept on separate pages. A mechanism here is the canonical arrow pushing for a class, run on real structures and labelled rule-derived. It is not evidence, and this record is not a mechanism.