HuagongsheHuagongshe Chemistry Print Report · For research reference only
Malonic Acid → 1,3-Dioxane-4,6-dione, 2-methyl-2-(2-phenylethyl)-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Malonic Acid | HCID 867 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Benzyl acetone | HCID 17355 | — |
| Solvent | Water | HCID 962 | — |
| Product | 1,3-Dioxane-4,6-dione, 2-methyl-2-(2-phenylethyl)- | HCID 11975787 | — |
Reaction Steps
To a solution of malonic acid (56.7 g, 0.55 mol) and acetic anhydride (73 ml), sulfuric acid (2 ml) was added dropwise at 5°-10° C. and stirring was continued for 20 min at the same temperature. To this mixture, 4-phenyl-2-butanone (105 g, 0.7 mol) was added dropwise at 15°-20° C. and stirring was continued for 15 h at the same temperature. The reaction mixture was taken up into H2O, extracted with chloroform, then the organic extract was washed with H2O, dried over anhydrous MgSO4 and evaporated. The resultant solid was recrystallized from aqueous acetone to give the title compound as a white amorphous solid; yield: 68.0 g; mp. 63.0°-65.0° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05250669 |
| Source dataset | uspto-grants-1993_10 |
| ORD ID | ord-8fa70bbbf4f04ee0959b0faa5a5cbbb4 |
| Source note | uspto-grants-1993_10 |