HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Malonate → HCID 71283960, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Malonate | HCID 7761 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 1,2,3-Trifluoro-5-nitrobenzene | HCID 2782793 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 71283960 | HCID 71283960 | 94.6% |
Reaction Steps
Diethyl malonate (44.8 g, 280 mmol) was added to a suspension of sodium hydride (60%, oil, 28.0 g, 700 mmol) in THF (280 mL) at 0° C., and the mixture was stirred at room temperature for 1 hr. Then, 1,2,3-trifluoro-5-nitrobenzene (24.79 g, 140 mmol) was added thereto at 0° C., and the mixture was stirred at room temperature for 2 hr. To the reaction mixture was added aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate (×2). The organic layer was washed with brine, and dried over magnesium sulfate, and the solvent was evaporated under reduced pressure to give diethyl 2,6-difluoro-4-nitrophenylmalonate (42 g) as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09365520B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-64793b4caeeb4c15adb700443bf1a7a3 |
| Source note | uspto-grants-2016_06 |