HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → Ethyl 1-acetylcyclopropane-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | Ethyl Acetoacetate | HCID 8868 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | Ethyl 1-acetylcyclopropane-1-carboxylate | HCID 234183 | 33.9% |
Reaction Steps
A total of 165.6 g of potassium carbonate, 390.0 g of 1,2-dichloroethane, 234.0 g of N,N-dimethylacetamide, 5.0 g of potassium iodide, and 78.0 g of ethyl acetoacetate were mixed, followed by a reaction at 100° C. for 4 hours. The reaction mixture was cooled to room temperature and was filtrated, the resulting filtrate was washed with two portions of 5% by weight hydrochloric acid, and the organic layer was washed with water. The organic layer was then concentrated under a reduced pressure to distill off 1,2-dichloroethane, was subjected to distillation under a reduced pressure and thereby yielded 31.7 g of ethyl 1-acetyl-1-cyclopropanecarboxylate as a colorless liquid as a fraction at 80° C./20 mmHg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06613935B2 |
| Source dataset | uspto-grants-2003_09 |
| ORD ID | ord-e881e2aefc1844d19c6935a49283d94e |
| Source note | uspto-grants-2003_09 |