HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl (ethoxymethylene)malonate → 288251-62-7
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl (ethoxymethylene)malonate | HCID 6871 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Fluorophenylhydrazine hydrochloride | HCID 69981 | — |
| Solvent | Water | HCID 962 | — |
| Product | 288251-62-7 | HCID 22228038 | 48.8% |
Reaction Steps
To a suspension of (4-fluorophenyl)hydrazine•hydrochloride (3 g, 18 mmol) and water (75 mL) were added potassium carbonate (5.6 g, 40 mmol) and diethyl ethoxymethylenemalonate (4.8 g, 22 mmol), and the mixture was heated under reflux for 7 hr. After cooling to room temperature, the mixture was washed with ethyl acetate. 6N Aqueous hydrochloric acid solution was added to the separated aqueous layer under ice-cooling. The precipitated solid was collected by filtration, washed with water and ethyl acetate/hexane (1/10), and dried under reduced pressure to give the title compound (2.2 g, 48%) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08445509B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-49e35ae4005d40fca09197084167709c |
| Source note | uspto-grants-2013_05 |