HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → (2,6-difluorophenyl)-N-[5-(2-fluoro-6-methylbenzo[b]furan-5-yl)(2-pyridyl)]carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,6-Difluorobenzoyl chloride | HCID 87438 | — |
| Reactant | Sodium bicarbonate methylene chloride | HCID 23716255 | — |
| Reactant | 5-(2-Fluoro-6-methylbenzo[b]furan-5-yl)-2-pyridylamine | HCID 58487414 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (2,6-difluorophenyl)-N-[5-(2-fluoro-6-methylbenzo[b]furan-5-yl)(2-pyridyl)]carboxamide | HCID 58487169 | 68.6% |
Reaction Steps
To a solution of 5-(2-fluoro-6-methylbenzo[b]furan-5-yl)-2-pyridylamine (231) (23 mg, 0.095 mmol) in 3 ml DCM was added 2,6-difluorobenzoyl chloride (36 μl, 3 eq) followed by addition of DIEA (149 μl). The resulting solution was stirred overnight at r.t. The reaction mixture was worked up with aq. NaHCO3/DCM. DCM phase was washed with brine, concentrated to dryness. The residue was dissolved in 3 ml THF/MeOH/H2O (5:4:1) and stirred with 1N NaOH (200 μl) at r.t. for 2 h before worked up with EA/aq. NaHCO3. Silica gel flash chromatography furnished (2,6-difluorophenyl)-N-[5-(2-fluoro-6-methylbenzo[b]furan-5-yl)(2-pyridyl)]carboxamide (223) (24.9 mg, yield: 68.6%, purity>95%) as white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08980629B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-30e47dc5e1ff431eab13f880607c099b |
| Source note | uspto-grants-2015_03 |