HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 18393045, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Iodobenzyl bromide | HCID 954258 | — |
| Reactant | HCID 1221966 | HCID 1221966 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 18393045 | HCID 18393045 | 76.9% |
Reaction Steps
To a solution of 5-ethyl-2-trifluoroacetylamino-1,3,4-thiadiazole (22.5 g) and 4-iodobenzyl bromide (32.7 g) in N,N-dimethylformamide (100 ml) was added potassium carbonate (13.8 g), followed by stirring at room temperature overnight. To the reaction mixture, ethyl acetate (500 ml) was added. The resulting mixture was washed three times with 10% aqueous citric acid solution, followed by drying over anhydrous magnesium sulfate. The solvent was then distilled off. The oily substance so obtained was separated by column chromatography on silica gel. The crystals so obtained were dispersed in n-hexane, collected by filtration and then dried, whereby 33.9 g of the title compound was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05965738 |
| Source dataset | uspto-grants-1999_10 |
| ORD ID | ord-b5c2e6d6d2d448569fd4fe0f04ba8076 |
| Source note | uspto-grants-1999_10 |