HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 18388329, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 18388310 | HCID 18388310 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 18388329 | HCID 18388329 | 89.8% |
Reaction Steps
Ethyl 4,5,6,7-tetrahydro-3-methylthio-4-oxobenzo[c]furan-1-carboxylate (4.26 g) was dissolved in chloroform (75 ml); a solution of bromine (2.73 g) in chloroform (5 ml) was added dropwise at room temperature over a period of 10 minutes. After the reaction mixture was stirred at room temperature for 30 minutes, it was washed with a 2% aqueous solution of sodium sulfite (100 ml), water, a saturated aqueous solution of sodium hydrogen carbonate and water in that order, and dried (MgSO4), after which the solvent was distilled off to yield ethyl 5-bromo-4,5,6,7-tetrahydro-3-methylthio-4-oxobenzo[c]furan-1-carboxylate (5.01 g, 89.8%), which was then recrystallized from ethyl acetate-hexane. Colorless needles. Melting point 130-131° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06489351B1 |
| Source dataset | uspto-grants-2002_12 |
| ORD ID | ord-ae3f979750cb445fb9a5d58556a17f62 |
| Source note | uspto-grants-2002_12 |