HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178468954, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Ethyl 4-(bromomethyl)benzoate | HCID 954261 | — |
| Reactant | HCID 178418558 | HCID 178418558 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178468954 | HCID 178468954 | 35.8% |
Reaction Steps
To a mixture of 1.2 g of 2,5-dimercapto-1,3,4-thiadiazole, 1.1 g of anhydrous potassium carbonate and 10 ml of N,N-dimethylformamide was added 0.5 g of ethyl p-(bromomethyl)benzoate followed by stirring at room temperature for 3 hours. The reaction mixture was made acidic with diluted hydrochloric acid and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was applied to silica gel column chromatography followed by eluting with a solvent mixture of toluene-ethyl acetate (9:1). The thus obtained crystals were recrystallized from toluene-n-hexane to give 230 mg of ethyl p-[(5-mercapto-1,3,4-thiadiazol-2-yl)thiomethyl]benzoate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04933348 |
| Source dataset | uspto-grants-1990_06 |
| ORD ID | ord-29ea9e62a6aa41f485bbf1ef84eac80f |
| Source note | uspto-grants-1990_06 |