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Buchwald–Hartwig amination, record ord-cf737b8f3d9340aca6130b04f75e7c21

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
Reactant1,4-DibromobenzeneC₆H₄Br₂
Reactant1-Piperazineacetic acid, methyl esterC₇H₁₄N₂O₂
ReagentCesium carbonateCCs₂O₃
CatalystBinap, (A+-)-C₄₄H₃₂P₂
CatalystBis(dibenzylideneacetone)palladiumC₅₁H₄₂O₃Pd₂
Solvent1,4-DioxaneC₄H₈O₂
ProductMethyl 2-(4-(4-bromophenyl)piperazin-1-yl)acetateC₁₃H₁₇BrN₂O₂0%

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
85 °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 Methyl 2-(4-(4-bromophenyl)piperazin-1-yl)acetate.

Procedure

Copied from the source record, unedited

In a reaction vial, 1,4-dibromobenzene (0.373 g, 1.58 mmol), methyl 2-(piperazin-1-yl)acetate (0.100 g, 0.63 mmol), CS2CO3 (0.309 g, 0.95 mmol), and BINAP (0.024 g, 0.04 mmol) were taken up in 1,4-dioxane (1.5 ml). Argon was bubbled through the solution for 1 minute. Pd2(dba)3 (0.012 g, 0.01 mmol) was added, followed by additional purging with argon. The vial was capped and placed on the heater-shaker. The reaction was stirred (450 rpm) at 100 °C overnight. LC/MS at this point did not indicate any formation of the dp. Experiment not progressed.

The source

This record comes from experimental reaction archive (ord-cf737b8f3d9340aca6130b04f75e7c21). Open the source and check it against what is on this page.

  • experimental reaction archive record ord-cf737b8f3d9340aca6130b04f75e7c21 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.