HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Iodide → (+/-)-[1-(2,4-Dichloro-pyrimidin-5-yl)-ethyl]-(4-methoxy-phenyl)-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | P-Anisidine | HCID 7732 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | (+/-)-2,4-Dichloro-5-(1-bromoethyl)-pyrimidine | HCID 21908975 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | (+/-)-[1-(2,4-Dichloro-pyrimidin-5-yl)-ethyl]-(4-methoxy-phenyl)-amine | HCID 10086026 | — |
Reaction Steps
(±)-2,4-Dichloro-5-(1-bromoethyl)-pyrimidine (1.97 g; 7.70 mmol) (from Example 1c supra) was dissolved in acetonitrile (21 mL). p-Anisidine (0.95 g; 7.70 mmol) (Aldrich), potassium carbonate (1.17 g; 8.48 mmol) and potassium iodide (0.32 g; 1.93 mmol) were added and the mixture was stirred at room temperature. After 16 hours, the mixture was partitioned between ethyl acetate and water. The organic phase was washed with water and brine, dried over anhydrous sodium sulfate, filtered and concentrated. Purification by flash chromatography (Biotage 40M, 20:80 to 25:75 ethyl acetate-hexanes gradient) gave (±)-[1-(2,4-dichloro-pyrimidin-5-yl)-ethyl]-(4-methoxy-phenyl)-amine. (Yield 1.82 g; 76.3%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07112676B2 |
| Source dataset | uspto-grants-2006_09 |
| ORD ID | ord-9a17983790d3494ba063a4d0181ed180 |
| Source note | uspto-grants-2006_09 |