HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Oxalate → HCID 67524928, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Oxalate | HCID 7268 | — |
| Reactant | 3',4',5'-Trimethoxyacetophenone | HCID 14345 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67524928 | HCID 67524928 | — |
Reaction Steps
3′,4′,5′-Trimethoxyacetophenone (12.0 g) was dissolved in THF (50 mL), and potassium tert-butoxide (8.16 g) was added to the solution at 0° C. A THF solution (20 mL) of diethyl oxalate (11.4 g) was then added dropwise to the mixture, and the resultant mixture was stirred for 1 hour. A saturated aqueous solution of ammonium chloride was added to the reaction mixture, and the resultant mixture was extracted with ethyl acetate. The resultant organic layer was washed with saturated brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resultant crude crystals were recrystallized from chloroform-hexane to obtain the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06472386B1 |
| Source dataset | uspto-grants-2002_10 |
| ORD ID | ord-86694bff3509438ab1507b2d39e12aa1 |
| Source note | uspto-grants-2002_10 |