HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfoxide → HCID 59427282, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 4-Chloroquinoline-7-carbonitrile | HCID 22054581 | — |
| Reactant | HCID 136131615 | HCID 136131615 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 59427282 | HCID 59427282 | — |
Reaction Steps
A microwave reaction vial was charged with 4-chloroquinoline-7-carbonitrile (97.1 mg, 0.515 mmol), 4-(4-ethyl-6-phenylpyridazin-3-ylamino)phenol (150 mg, 0.515 mmol), cesium carbonate (252 mg, 0.772 mmol) and 2.6 mL of DMSO. The vial was sealed, and the reaction mixture was irradiated in the microwave at 150° C. for 15 min. Upon cooling the mixture was poured into water and the resulting solids were filtered and washed with water. The crude solids were dissolved in 90/10/1 CH2Cl2/MeOH/NH4OH and purified by silica gel chromatography, 5-100% 90/10/1: CH2Cl2 over 25 min which provided 4-(4-(4-ethyl-6-phenylpyridazin-3-ylamino)phenoxy)quinoline-7-carboxamide as a tan solid. MS m/z=462 [M+H]+. Calc'd for C28H23N3O2: 461.52.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08557816B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-02006fbc5cdf49e994d968e731efc9e8 |
| Source note | uspto-grants-2013_10 |