HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 59676099, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 18-Crown-6 | HCID 28557 | — |
| Reactant | HCID 59676097 | HCID 59676097 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59676099 | HCID 59676099 | — |
Reaction Steps
9-Methoxy-6,7-dihydro-12H-5-thia-12-aza-dibenzo[a,e]azulene (57 mg, 0.203 mmoL) in DMF (2 mL) was treated with KO2 (58 mg, 0.811 mmoL) and 18-Crown-6 (54 mg, 0.203) and the reaction mixture was stirred at room temperature for 6 hours. Water was added to quench the reaction. The mixture was then partitioned between EtOAc and saturated NH4Cl. The aqueous phase was extracted two times with EtOAc. The organic layer from each extraction was combined, washed with water, brine, dried over anhydrous Na2SO4, filtered and concentrated to yield a brown oil. The crude material (the oil) was then purified by column chromatography (silica gel, 1:1 hexanes:EtOAc as eluent) to yield the title compound as a brown solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08318766B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-4c8f5e4aa977498695da718a23bcfc68 |
| Source note | uspto-grants-2012_11 |