HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 21995659, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 18472606 | HCID 18472606 | — |
| Reactant | Ethanol toluene water | HCID 86587398 | — |
| Reactant | HCID 86756176 | HCID 86756176 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Product | HCID 21995659 | HCID 21995659 | — |
Reaction Steps
Under argon atmosphere, a mixture of methyl 7-bromo-2,3-dihydro-1-benzothiepine-4-carboxylate (0.80 g), 4-isopropylphenyl borate (0.44 g) and potassium carbonate (0.67 g) in toluene/ethanol/water (30/3/3 ml) was stirred at room temperature for 1 hour. To the mixture was added tetrakistriphenylphosphinepalladium (0.14 g), and the mixture was refluxed for 20 hours, cooled, extracted with ethyl acetate, washed with saturated brine, dried with magnesium sulfate and concentrated under reduced pressure. The residue was purified with column chromatography (ethyl acetate/hexane=1:2) to give pale yellow crystals of methyl 7-(4-isopropylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (774.7 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06235771B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-8bfd0adb2e644eb6bc8086f0f324dee3 |
| Source note | uspto-grants-2001_05 |