HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 3-Hydroxy-2,2-dimethylpropyl 2,2,4-trimethyl-3-oxopentanoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2,2,4,4-Tetramethyl-1,3-cyclobutanedione | HCID 13617 | — |
| Reactant | Neopentyl glycol | HCID 31344 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-Hydroxy-2,2-dimethylpropyl 2,2,4-trimethyl-3-oxopentanoate | HCID 86667140 | 100% |
Reaction Steps
To a 1-liter round bottom flask was charged 2,2,4,4-tetramethyl-1,3-cyclobutanedione (140.2 g, 1.0 moles), neopentyl glycol (208.3 g, 2.0 moles), potassium carbonate (138 g, 1.0 moles) and 500 grams methylene chloride. The batch was heated to reflux for 3 hours then cooled and clarified to remove salts. Methylene chloride was removed with a rotary evaporator and 250 grams of toluene added. The organic layer was washed with 6×50 mL of demineralized water and dried with anhydrous sodium sulfate. Toluene was removed at 3 mmHg and 75° C. to provide 244.4 g of product. GC assay of the product was 96.2%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09029451B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-5cca6038af9142acab008566e836fa34 |
| Source note | uspto-grants-2015_05 |