HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 58866169, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 58866182 | HCID 58866182 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58866169 | HCID 58866169 | 3,585% |
Reaction Steps
The above compound (4) (7.4 g) was dissolved in DMF (80 mL) and DMP (17.6 g) and p-toluenesulfonic acid monohydrate (70 mg) were added, and then the mixture was stirred overnight at room temperature and further stirred at 60° C. for 1.5 hours. To the reaction solution was added ethyl acetate (150 mL) and, after washing with an aqueous saturated sodium hydrogencarbonate solution and saturated saline (×3), the organic layer was dried over magnesium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel medium pressure column chromatography (ethyl acetate:cyclohexane=1:3→1:2→1:1) to obtain the titled compound (6.3 g) as a syrup.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07223779B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-8045ede264134304b4a2cb7714c93c05 |
| Source note | uspto-grants-2007_05 |