HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,6-Dichloro-isonicotinoyl chloride → 6-(2,6-dichloro-pyridine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,6-Dichloro-isonicotinoyl chloride | HCID 2781643 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Reactant | 4-Methyl-3H-benzooxazol-2-one | HCID 12709336 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 6-(2,6-dichloro-pyridine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one | HCID 58181212 | — |
Reaction Steps
3.00 g (14.3 mmol) 2,6-dichloropyridine-4-carboxylic acid chloride, 1.80 g (11.0 mmol) 4-methyl-3H-benzoxazol-2-one and 9.47 g (71.0 mmol) aluminium trichloride were combined and heated for 2 h to 125° C. with stirring. Then the mixture was decomposed with ice water and EtOAc and the phases were separated. The aqueous phase was extracted several times with EtOAc. The organic phases were combined, dried on sodium sulphate, filtered and the filtrate was evaporated down i. vac. The residue was triturated with diethyl ether, the precipitate was suction filtered and dried i. vac.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08629137B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-d8a2718c0911453f9d47a4de7cf71a7f |
| Source note | uspto-grants-2014_01 |