HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → 5-(2-fluorophenyl)-2,2-dimethyl-6-methyl-4H-1,3-dioxin-4-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Acetyl(2-fluorophenyl)acetic acid | HCID 3023024 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | 5-(2-fluorophenyl)-2,2-dimethyl-6-methyl-4H-1,3-dioxin-4-one | HCID 15300846 | — |
Reaction Steps
A mixture of 2-(2-fluorophenyl)acetoacetic acid (5.1 g), acetone (4.2 ml), and acetic anhydride (5.4 ml) was kept at -20° C. and concentrated sulfuric acid (0.3 ml) was added thereto. This was kept at -15° C. and the reaction was carried out for 48 hours. The reaction mixture was added to an aqueous 10 % sodium carbonate solution (150 ml) which was ice-cooled, and the mixture was stirred for a short time at room temperature. White crystals which formed were collected by filtration, and washed well with water and then with hexane. The crystals obtained were dried well under reduced pressure to obtain the captioned compound (5.2 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05436224 |
| Source dataset | uspto-grants-1995_07 |
| ORD ID | ord-bdc3e776827c407685d5ec95f971d9c4 |
| Source note | uspto-grants-1995_07 |