HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 178419912, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Chroman-4-ol | HCID 92890 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 178527894 | HCID 178527894 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178419912 | HCID 178419912 | 47.2% |
Reaction Steps
To a mixture of triphosgene (95 mg) and dichloromethane (4 ml), with stirring, were added pyridine (82 μl) and 4-chromanol (150 mg) in this order with cooling it on an ice bath. Additional pyridine (82 μl) was added, and the reaction mixture was stirred at room temperature for 2 hours. The reaction solution was added to a mixture of 3-mercapto-1H-1,2,4-triazole (110 mg), anhydrous potassium carbonate (200 mg) and N,N-dimethylformamide (2 ml), and stirred overnight. The reaction solution was washed with water, followed by saturated aqueous sodium chloride solution, and concentrated. The residue was subjected to a silica-gel column chromatography with 50% ethyl acetate/hexane to yield the title compound (110 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07238720B2 |
| Source dataset | uspto-grants-2007_07 |
| ORD ID | ord-347620f152da4b16bd2c6f0d697eaea6 |
| Source note | uspto-grants-2007_07 |