HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 178508870, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | methyl 5-oxo-6,7,8,9-tetrahydro-5H-benzo[7]annulene-6-carboxylate | HCID 10104791 | — |
| Reactant | CID 21864146 | HCID 21864146 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178508870 | HCID 178508870 | 68.4% |
Reaction Steps
A solution of the product from Example 4A (4.2 g, est. 18 mmol), guanidine chloride (7.1 g, 72.8 mmol), and K2CO3 (10.8 g, 78 mmol) in DMF (30 mL) was heated to 125° C. for 3 hours. The mixture was cooled and the solids were removed by filtration. The solids were washed with EtOAc. The combined filtrates were concentrated under reduced pressure and the residue was passed through silica gel pad eluting with EtOAc:hexanes (8:2) and then with MeOH:EtOAc:CH2Cl2 (10:45:45) to provide the title compound as a white solid (2.8 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07985745B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-e935b28794954a5990241555437b808b |
| Source note | uspto-grants-2011_07 |