HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → Ethyl 2-(1,3,5-triethylphenyl)-2-oxoacetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Diethyl Oxalate | HCID 7268 | — |
| Reactant | HCID 178436339 | HCID 178436339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Ethyl 2-(1,3,5-triethylphenyl)-2-oxoacetate | HCID 66691385 | — |
Reaction Steps
On the other hand, to a 3 L volume four-necked flask, diethyl oxalate (295 g) and tetrahydrofuran (anhydrous) (350 ml) were added under a nitrogen atmosphere and cooled on ice-bath. The above mentioned solution of 1,3,5-triethylphenylmagnesium bromide in tetrahydrofuran was added thereto with keeping the temperature below 10° C. The resulting mixture was stirred at room temperature for 2 hours. The pH of the mixture was adjusted to less than 2 with 20 w/w % of sulfuric acid under ice-cooling. The mixture was extracted with toluene. The organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give 495.3 g of ethyl 2-(1,3,5-triethylphenyl)-2-oxoacetate (9-b).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09040709B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-cd290c5279654a0b87358327b327b6d4 |
| Source note | uspto-grants-2015_05 |