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Buchwald–Hartwig amination, record ord-dc56e46e611f4db1889616d29baeeb5f

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

verified record0% 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-Bromo-1-benzofuran-2-carboxamideC₉H₆BrNO₂
ReactantPiperazineC₄H₁₀N₂
ReagentCesium carbonateCCs₂O₃
CatalystBinap, (A+-)-C₄₄H₃₂P₂
CatalystBis(dibenzylideneacetone)palladiumC₅₁H₄₂O₃Pd₂
SolventTetrahydrofuranC₄H₈O
Product4-Piperazin-1-yl-1-benzofuran-2-carboxamideC₁₃H₁₅N₃O₂0%

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
70 °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

  • 0% of 4-Piperazin-1-yl-1-benzofuran-2-carboxamide.

Procedure

Copied from the source record, unedited

The crude product from EN03731-54-001, 4-bromobenzofuran-2-carboxamide (0.600 g, 2.5 mmol), was dissolved in THF (18 mL) and water (18.00 mL). To this mixture were added piperazine (1.077 g, 12.50 mmol), Cesium carbonate (1.629 g, 5.00 mmol), Tris(dibenzylideneacetone)dipalladium(0) (0.114 g, 0.13 mmol) and rac-2,2'-Bis(diphenylphosphino)-1,1'-binaphthyl (0.156 g, 0.25 mmol) and the reaction was heated at 70 °C over night. 2010-04-13 No product was detected. The reaction mixture was filtered and solvents were removed in vacuo. The residue was partitioned between methylene chloride and water. The organic layer was washed with 1M HCl(aq), dired with sodium sulfate, filtered, concentrated and purified by flash chromatography(Isolute Si 70g, methylene chloride: methanol; 97:3). No product cou

The source

This record comes from experimental reaction archive (ord-dc56e46e611f4db1889616d29baeeb5f). Open the source and check it against what is on this page.

  • experimental reaction archive record ord-dc56e46e611f4db1889616d29baeeb5f 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.