HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22032251, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2-Methoxyethanol | HCID 8019 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2,4-Difluoroacetophenone | HCID 67770 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22032251 | HCID 22032251 | 69.6% |
Reaction Steps
A solution of 1.75 g 2-methoxy ethanol in tetrahydrofuran (23 mL) was added dropwise to a suspension of 0.84 g of 60% sodium hydride in tetrahydrofuran (21 mL), and subsequently a solution of 3.0 g 2′,4′-difluoroacetophenone in tetrahydrofuran (19 mL) was added dropwise thereto. The temperature of the mixture was increased to room temperature, then the mixture was stirred for 24 hours, water was carefully added thereto, and the reaction mixture was extracted with ethyl acetate. The organic layer was washed with brine and then dried over anhydrous sodium sulfate, the solvent was removed, and the resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give 2.84 g of the title compound (yellow oil).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07074801B1 |
| Source dataset | uspto-grants-2006_07 |
| ORD ID | ord-f1c2816f2f184ef9a353812df19c64f4 |
| Source note | uspto-grants-2006_07 |