HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Fluorobenzoyl chloride → HCID 58486713, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Fluorobenzoyl chloride | HCID 9808 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Sodium bicarbonate methylene chloride | HCID 23716255 | — |
| Reactant | HCID 58486925 | HCID 58486925 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58486713 | HCID 58486713 | 66.4% |
Reaction Steps
To a solution of 5-(5-chloro-2,3-dihydrobenzo[3,4-b]furan-6-yl)-2-pyridylamine (151) (15 mg, 0.06 mmol) in 1 ml DCM was added 2-fluorobenzoyl chloride (11 μl, 0.088 mmol) followed by addition of DIEA (52 μl). The resulting solution was stirred at r.t. for overnight. The reaction mixture was worked up with aq. NaHCO3/DCM. DCM phase was washed with brine, concentrated to dryness. The residue was dissolved in 1 ml THF/MeOH/H2O (5:4:1) and stirred with 1N NaOH (120 μl) at r.t. for 2 h and before worked up with EA/aq. NaHCO3. Silica gel flash chromatography furnished N-[5-(5-chloro(2,3-dihydrobenzo[3,4-b]furan-6-yl))(2-pyridyl)](2-fluorophenyl)carboxamide (153) (14.7 mg, yield: 66.4%, purity>90%) as white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08980629B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-252ef06053dd4fde9d45e6f6f9d50a24 |
| Source note | uspto-grants-2015_03 |