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Buchwald–Hartwig amination, record ord-8dc05311ad5340e693477414d5741a5e

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
ReactantO=c1cc(N2CCOCC2)oc2c(-c3ccc(I)c4c3sc3ccccc34)cccc12C₂₅H₁₈INO₃S
Reactant1-EthylpiperazineC₆H₁₄N₂
ReagentCesium carbonateCCs₂O₃
Catalyst1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)C₃₉H₃₂OP₂
CatalystBis(dibenzylideneacetone)palladiumC₅₁H₄₂O₃Pd₂
Solvent1,4-DioxaneC₄H₈O₂
Product8-[1-(4-Ethylpiperazin-1-yl)dibenzothiophen-4-yl]-2-morpholin-4-ylchromen-4-oneC₃₁H₃₁N₃O₃S0%

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
130 °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 8-[1-(4-Ethylpiperazin-1-yl)dibenzothiophen-4-yl]-2-morpholin-4-ylchromen-4-one.

Procedure

Copied from the source record, unedited

8-(1-iododibenzo[b,d]thiophen-4-yl)-2-morpholino-4H-chromen-4-one (20 mg, 0.04 mmol), 1-ethylpiperazine (9.42 µl, 0.07 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (2.145 mg, 3.71 µmol), TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM (0.849 mg, 0.93 µmol) and 2,3,4,6,7,8,9,10-octahydropyrimido[1,2-a]azepine (16.62 µl, 0.11 mmol) were suspended in dioxane (250 µl) and sealed into a microwave tube. The reaction was degased, purged with argon and heated to 130 °C over a period of 45 minutes in the microwave reactor. No reaction.

The source

This record comes from experimental reaction archive (ord-8dc05311ad5340e693477414d5741a5e). Open the source and check it against what is on this page.

  • experimental reaction archive record ord-8dc05311ad5340e693477414d5741a5e 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.