HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 72211834, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Phosphorus pentachloride | HCID 24819 | — |
| Reactant | (3-Fluoro-5-methoxyphenyl)methanol | HCID 26985456 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | HCID 72211834 | HCID 72211834 | 55.4% |
Reaction Steps
To a solution of (3-fluoro-5-methoxyphenyl)methanol (4.9 g, 30 mmol) in CCl4 (50 mL), PCl5 (13 g, 60 mmol) was added. The mixture was stirred at room temperature for 1 h. To this mixture, saturated Na2CO3 solution was slowly added until pH was adjusted to 7˜8. The mixture was extracted with DCM (3×15 mL), and the organic phase was concentrated to give a colorless oil, which was purified by silica-gel column chromatography (100% petroleum ether) to give 2.9 g of 1-(chloromethyl)-3-fluoro-5-methoxybenzene. 1H NMR (CDCl3): δ 6.68-6.72 (m, 2H), 6.54-6.59 (m, 1H), 4.51 (s, 2H), 3.81 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09078871B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-44e6157ebf9c43eda45320740a20de6f |
| Source note | uspto-grants-2015_07 |