HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloride → HCID 68421745, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloride | HCID 312 | — |
| Reactant | N,N-Dimethylaniline | HCID 949 | — |
| Reactant | HCID 178486806 | HCID 178486806 | — |
| Solvent | Phosphorus oxychloride | HCID 24813 | — |
| Product | HCID 68421745 | HCID 68421745 | — |
Reaction Steps
5-(4-(6,7-Dimethoxyquinolin-4-yloxy)-3-fluorophenyl)-2-hydroxy-3-methyl-3H-pyrimidin-4-one (Step 2, 678.8 mg, 1.605 mmol) was dissolved in POCl3 (16 mL) and N,N-dimethylaniline (1.6 ml) and heated at 125° C. for 8.5 h then cooled to RT and stirred overnight. The reaction was concentrated, diluted with CH2Cl2 (125 mL) and washed with saturated NaHCO3 (25 mL, 17 mL). The organic layer was dried over Na2SO4, filtered, and concentrated. Because of the propensity of title compound to hydrolysis, the crude chloride was used for the next reaction.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07652009B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-21ca7e16da6c46e28be1aa058b827bc1 |
| Source note | uspto-grants-2010_01 |