HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 59287328, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Bromo-3-fluorophenol | HCID 2779153 | — |
| Reactant | 4-Bromo-2,6-dimethylpyridine | HCID 13081735 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 59287328 | HCID 59287328 | 73.8% |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
A mixture of 4-bromo-2,6-dimethyl-pyridine (1 g, 5.4 mmol), 4-bromo-3-fluoro-phenol (0.59 g, 5.4 mmol), and potassium carbonate (0.89 g, 6.4 mmol) in xylenes (2 ml) was heated at 150° C. (oil bath temperature) in a sealed tube for 48 hours. After cooling to room temperature the mixture was diluted with EtOAc and filtered through a diatomaceous earth pad. The filtrate was evaporated till dryness and the crude product thus obtained was purified by column chromatography (silica gel; DCM to DCM/EtOAc up to 10% as eluent). The desired fractions were collected and evaporated in vacuo to yield intermediate 17 (1.18 g, 72%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09067891B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-9f310a2217ea4c70a0ab73ee85f10ecc |
| Source note | uspto-grants-2015_06 |