Skip to the content
Browse the library

Buchwald–Hartwig amination: 4-Bromophenol → tert-butyl (3R)-4-(4-hydroxyphenyl)-3-methylpiperazine-1-carboxylate

0% yield, run at 100 °C, as recorded by experimental reaction archive. The written procedure is below.

verified record, 0% yield recorded, Not balanced as written, From experimental reaction archive

Reagents, catalysts and solvents are in the table below.

The atoms, from reactants to products

CCCNCOOCCCCCCNCCCCOCCBr
Reactants · 1/6
breakingformingbond order changesmapped atom that changes

Drawn from the record's atom map: which bonds break and which form between the reactants and products the source listed. It shows a change in connectivity, not a simulated trajectory and not a mechanism.

What was in the flask

RoleSpeciesFormulaYield
Reactant4-BromophenolC₆H₅BrO—
Reactant(R)-1-Boc-3-methylpiperazineC₁₀H₂₀N₂O₂—
Reagentpotassium 2-methylpropan-2-olateC₄H₉KO—
CatalystTris(1,1-dimethylethyl)phosphineC₁₂H₂₇P—
CatalystBis(tri-tert-butylphosphine)palladium(0)C₂₄H₅₄P₂Pd—
SolventTetrahydrofuranC₄H₈O—
Producttert-butyl (3R)-4-(4-hydroxyphenyl)-3-methylpiperazine-1-carboxylateC₁₆H₂₄N₂O₃0%

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
100 °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 tert-butyl (3R)-4-(4-hydroxyphenyl)-3-methylpiperazine-1-carboxylate.

Procedure

Copied from the source record, unedited

A mixture of (R)-tert-butyl 3-methylpiperazine-1-carboxylate (0.025 g, 0.12 mmol), 4-bromophenol (0.043 g, 0.25 mmol), bis(tri-t- butylphosphine)palladium(0) (6.38 mg, 0.01 mmol) and [Reactants] in THF (2 mL) was flushed with nitrogen and sealed into a microwave tube. The reaction was heated to 100 °C for 20 minutes in the microwave reactor and cooled to RT. No trace of desired product by LCMS. The reaction was not progressed further.

The source

This record comes from experimental reaction archive (ord-512d2d9fb0454cb39e6db5113f92b34b). Open the source and check it against what is on this page.

  • experimental reaction archive record ord-512d2d9fb0454cb39e6db5113f92b34b 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.