HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 19770953, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Ethyl propiolate | HCID 12182 | — |
| Reactant | 1-Amino-2-ethylpyridin-1-ium iodide | HCID 15201891 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19770953 | HCID 19770953 | 24% |
Reaction Steps
Next, 2.2 g (20.8 mmol) of Na2CO3 were added to a solution of 4.5 g (18.0 mmol) of 1-amino-2-ethylpyridinium iodide in 20 ml of DMF, followed by stirring at room temperature for 1 hour. Ethyl propiolate (3.6 g; 36.7 mmol) was added further, followed by stirring at room temperature for 20 hours. The solvent of the reaction mixture was distilled off. Water was added to the residue, followed by extraction with methylene chloride. After the methylene chloride layer was dried over Na2SO4, the solvent was distilled off and the residue was purified by chromatography on a silica gel column, whereby 0.93 g (4.3 mmol) of the title compound was obtained as crystals (yield: 24%-12% in two steps).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05200415 |
| Source dataset | uspto-grants-1993_04 |
| ORD ID | ord-a63bddb50345421b9532ee0b0f44ac78 |
| Source note | uspto-grants-1993_04 |