HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chlorobenzoyl chloride → N-[5-(5-chloro-2-methylbenzoxazol-6-yl)(2-pyridyl)](2-chlorophenyl)carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chlorobenzoyl chloride | HCID 69110 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Sodium bicarbonate methylene chloride | HCID 23716255 | — |
| Reactant | 5-(5-Chloro-2-methylbenzoxazol-6-yl)-2-pyridylamine | HCID 58487024 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-[5-(5-chloro-2-methylbenzoxazol-6-yl)(2-pyridyl)](2-chlorophenyl)carboxamide | HCID 58486904 | 71% |
Reaction Steps
To a solution of 5-(5-chlorob-2-methylenzoxazol-6-yl)-2-pyridylamine (36) (19 mg, 0.073 mmol) and 2 mg DMAP in 2 ml DCM was added 2-chlorobenzoyl chloride (19 μl, 0.14 mmol) followed by addition of DIEA (64 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 2 ml THF/MeOH/H2O (5:4:1) and stirred with 1N NaOH (140 μl) at r.t. for 1 h before worked up with EA/aq. NaHCO3. Silica gel flash chromatography furnished 20.6 mg 37 as pale yellow solid. (yield: 71%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08980629B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-b1eb9baebbc740c78b2cdb0ab7a57caa |
| Source note | uspto-grants-2015_03 |