HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 12535811, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Diethyl (ethoxymethylene)malonate | HCID 6871 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | HCID 20360326 | HCID 20360326 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 12535811 | HCID 12535811 | 67% |
Reaction Steps
2-Ethylthiobenzamidine hydrochloride (2.12 g., 10.0 mmoles) was added to a cooled (ice-water) solution of sodium (0.46 g., 20 mg.-atoms) in ethanol (12 ml.). To this mixture was added a solution of diethyl ethoxymethylenemalonate (2.16 g., 10.0 mmoles) in ethanol (4 ml.). The mixture was heated under reflux for 3.5 hours. The cooled mixture was poured into ice-water (400 ml.) and acidified to pH 6 with glacial acetic acid. The precipitate was collected and recrystallized from acetonitrile to give the title compound (2.04 g., 64.6%), m.p. 117°-120°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04082751 |
| Source dataset | uspto-grants-1978_04 |
| ORD ID | ord-a6130121747b45d78055f15f265ce7d3 |
| Source note | uspto-grants-1978_04 |