HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 17960600, compound → HCID 17960601, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 17960600 | HCID 17960600 | — |
| Catalyst | HCID 178418406 | HCID 178418406 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 17960601 | HCID 17960601 | 28.8% |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
To a solution of the title compound of Example 1, Step A (0.35 g, 1.71 mmol) in dimethylformamide (20 mL) was added activated manganese dioxide (4.46 g, 51.3 mmol) and the mixture was heated at 120° C. for 2 hours. After cooling, the mixture was diluted with ethyl acetate, filtered through a pad of Celite® and washed three times with water and once with a saturated solution of sodium chloride. The organic phase was dried (magnesium sulfate), concentrated and purified by flash column chromatography (silica gel, 60% then 80% ethyl ether in hexanes then ethyl ether) to give the title compound of Step A (0.1 g) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07375232B2 |
| Source dataset | uspto-grants-2008_05 |
| ORD ID | ord-f5c1fefdcc5b4486a58e3052e5941d4a |
| Source note | uspto-grants-2008_05 |