HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chlorobenzoyl chloride → N-[5-(5-chlorobenzoxazol-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-Chlorobenzoxazol-6-yl)-2-pyridylamine | HCID 58486911 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-[5-(5-chlorobenzoxazol-6-yl)(2-pyridyl)](2-chlorophenyl)carboxamide | HCID 58486794 | 49.2% |
Reaction Steps
To a solution of 5-(5-chlorobenzoxazol-6-yl)-2-pyridylamine (31) (23 mg, 0.09 mmol) and 2 mg DMAP in 2 ml DCM was added 2-chlorobenzoyl chloride (23 μl, 0.18 mmol) followed by addition of DIEA (94 μl). The resulting brown 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 (135 μl) at r.t. for 30 min before worked up with EA/aq. NaHCO3. Silica gel flash chromatography furnished 17 mg 32 as pale yellow solid. (yield: 49%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08546403B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-41986f35331e4674a847ba7a7480b993 |
| Source note | uspto-grants-2013_10 |