HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 24753314, compound → HCID 24753222, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 24753314 | HCID 24753314 | — |
| Solvent | Phosphorus oxychloride | HCID 24813 | — |
| Product | HCID 24753222 | HCID 24753222 | 85% |
Reaction Steps
A solution of 6-[(5-chloro-2-{[(4-chloro-2-fluorophenyl)methyl]oxy}phenyl)-methyl]-2-pyridinecarboxamide (115 mg) in phosphoryl chloride (1.25 ml) was stirred at 60° C. for 5 hours. Excess phosphoryl chloride was removed in vacuo and ethyl acetate (5 ml) added. The solution was washed with saturated sodium bicarbonate solution (5 ml), and the aqueous layer extracted with ethyl acetate (5 ml). The combined extracts were washed with brine (5 ml), dried (MgSO4) and concentrated in vacuo. The residue was purified by mass-directed autopreparation to afford the title compound (93 mg, 85%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07759369B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-940cdf843d77425da87999e1cf7ce068 |
| Source note | uspto-grants-2010_07 |