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.
The atoms, from reactants to products
What was in the flask
| Role | Species | Formula | Yield |
|---|---|---|---|
| Reactant | 4-Bromophenol | C₆H₅BrO | |
| Reactant | (R)-1-Boc-3-methylpiperazine | C₁₀H₂₀N₂O₂ | |
| Reagent | potassium 2-methylpropan-2-olate | C₄H₉KO | |
| Catalyst | Tris(1,1-dimethylethyl)phosphine | C₁₂H₂₇P | |
| Catalyst | Bis(tri-tert-butylphosphine)palladium(0) | C₂₄H₅₄P₂Pd | |
| Solvent | Tetrahydrofuran | C₄H₈O | |
| Product | tert-butyl (3R)-4-(4-hydroxyphenyl)-3-methylpiperazine-1-carboxylate | C₁₆H₂₄N₂O₃ | 0% |
Conditions
- Temperature
- 100 °C
Yield
- 0% of tert-butyl (3R)-4-(4-hydroxyphenyl)-3-methylpiperazine-1-carboxylate.
Other recorded runs with the same starting material
No other run in the library makes this product. These runs of the same class start from one of the same reactants, which is the nearest company this record has.
- tert-butyl (3R)-3-methyl-4-pyridin-3-ylpiperazine-1-carboxylate103%
- 4-(4-Methyl-1-piperazinyl)phenol51%
- (R)-4-(4-benzyloxyphenyl)-3-methylpiperazine-1-carboxylic acid tert-butyl ester32%
- 4-Morpholinophenol31%
- (R)-4-(4-benzyloxyphenyl)-3-methylpiperazine-1-carboxylic acid tert-butyl ester0%
- (R)-4-(4-benzyloxyphenyl)-3-methylpiperazine-1-carboxylic acid tert-butyl ester0%
- tert-butyl (3R)-3-methyl-4-pyridin-3-ylpiperazine-1-carboxylate0%
- tert-butyl (3R)-3-methyl-4-pyridin-3-ylpiperazine-1-carboxylate0%
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.
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.
Where to next
More Buchwald–Hartwig amination records
Other runs of this class, one page per distinct transformation.
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