HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pinacolone → 8-Methoxy-2,2-dimethyloctan-3,5-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pinacolone | HCID 6416 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Methyl 4-methoxybutanoate | HCID 542317 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | 8-Methoxy-2,2-dimethyloctan-3,5-dione | HCID 12991956 | 14% |
Reaction Steps
1.8 mol of sodium hydride was added to the solvent ethylene glycol dimethyl ether, and 1 mol of methyl 4-methoxybutanoate was added thereto and stirred at room temperature for 10 minutes. Then, 1.2 mol of t-butylmethylketone was added to the solution which was then stirred at 92° C. for 19 hours. Then, the solution was cooled to room temperature and quenched in 36% hydrochloric acid, after which water and dimethylether were added to and mixed with the solution, and water was removed therefrom. The resulting organic material was washed with 1 wt % sodium hydroxide and then with saturated saline and concentrated, and the residue was fractionated, thereby obtaining the intermediate 8-methoxy-2,2-dimethyloctan-3,5-dione at a yield of 14%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09359383B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-8a4bae9cbb284070b40cc4e87a517d92 |
| Source note | uspto-grants-2016_06 |