HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22335334, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2-Methoxyethanol | HCID 8019 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2,6-Difluoro-4-methoxybenzonitrile | HCID 2778772 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22335334 | HCID 22335334 | 84.4% |
Reaction Steps
Sodium hydride (60% in mineral oil, 0.88 g, 22 mmol) was added to 2-methoxyethanol (1.84 g, 24 mmol) in tetrahydrofuran (20 ml) and the mixture was stirred at room temperature for 20 minutes. 2,6-Difluoro-4-methoxy-benzonitrile (Mol. Cryst. Liq. Cryst. 1989, 172) (3.38 g, 20 mmol) was added and the mixture was stirred at room temperature for 1 hour. The reaction mixture was poured into water and the solution was extracted with dichloromethane (3×50 ml). The combined organic solutions were dried over magnesium sulphate and evaporated under reduced pressure. The residue was purified by chromatography on silica gel using methanol in dichloromethane as eluant (gradient from 0:100 to 3:97) to give the title compound (3.8 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06936619B2 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-6dbe55e922144499bb94d8ec2b197020 |
| Source note | uspto-grants-2005_08 |