HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Iodide → HCID 20485542, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | 2-Chloro-3',4'-dihydroxyacetophenone | HCID 66834 | — |
| Reactant | HCID 13150962 | HCID 13150962 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 20485542 | HCID 20485542 | 73.7% |
Reaction Steps
3,4-Dihydroxyphenacyl chloride (7 g) is added to a suspension of 5-(pyrrolidin-1-yl)-1,2-dithiol-3-thione (5.1 g) and sodium iodide (6.2 g) in acetone (90 cc), and the reaction mixture is kept under reflux for 1 hour. After cooling, the insoluble product is filtered off and washed successively with acetone (3×20 cc), with water (3×20 cc) and then with diethyl ether (3×20 cc). By recrystallisation of the resulting product from a dimethylformamide/methanol mixture (20/80 by volume; 600 cc) and then desolvation by stirring for 30 minutes in water (100 cc), N-[5-(3,4-dihydroxyphenacylthio)-1,2-dithiol-3-ylidene]-pyrrolidinium iodide hydrate (6.9 g), melting at about 130° C., is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04407797 |
| Source dataset | uspto-grants-1983_10 |
| ORD ID | ord-84b06199db3b4e80a761d4c9159decf0 |
| Source note | uspto-grants-1983_10 |