HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 11118300, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 11823569 | HCID 11823569 | — |
| Reactant | Water ethylacetate | HCID 22728543 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 11118300 | HCID 11118300 | 56.4% |
Reaction Conditions
| Temperature | 165 °C |
|---|
Reaction Steps
To a solution of N-(2-hydroxyphenyl)-2-bromo-4,5-dimethyl-3-thiophenecarboxamide (3.3 g) in dimethyl sulfoxide (50 ml) was added potassium carbonate (2.8 g) and the mixture was stirred at 160-170° C. for 20 minutes. The reaction system was cooled to room temperature and the reaction mixture was poured into water-ethyl acetate. The insoluble matter was filtrated and the filtrate was extracted with ethyl acetate, washed with water and dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1) to give 2,3-dimethylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.4 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06455521B1 |
| Source dataset | uspto-grants-2002_09 |
| ORD ID | ord-635b734c672b487e9d92a8150d9b9405 |
| Source note | uspto-grants-2002_09 |