HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 66823597, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 86663666 | HCID 86663666 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66823597 | HCID 66823597 | 65% |
Reaction Steps
To a solution of 2-(5-bromo-2-fluorophenyl)-4,4,6,6-tetramethyl-1,5-dioxaspiro[2.4]heptan-7-one (6.60 g, 19.30 mmol) in dichloromethane (8 ml) is added a second ice-cold solution of concentrated sulphuric acid (13.8 ml) dropwise, maintaining temperature below 5° C. The reaction mixture is stirred for a further 30 minutes, then quenched with distilled water (50 ml). After stirring for an additional 10 minutes the organics are removed in vacuo, and the resulting precipitate is filtered then triturated with water. After washing with hexanes the solid is dried to afford 4-(5-bromo-2-fluorophenyl)-2,2,6,6-tetramethylpyran-3,5-dione (4.30 g, 65%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08680299B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-0be27d0883c643f1a0e90d8cb1f005e8 |
| Source note | uspto-grants-2014_03 |