HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 3319467, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1,2-Cyclohexanedione | HCID 13006 | — |
| Reactant | Pyrylium, 2,4,6-triphenyl-, tetrafluoroborate(1-) | HCID 9930615 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 3319467 | HCID 3319467 | 79.3% |
Reaction Steps
A suspension of 13.51 g of 2,4,6-triphenylpyryliumtetrafluoroborate (34.1 mmol) and 4.78 g of cyclohexane-1,2-dione (42.6 mmol) is heated to boiling point in methanol, then a solution of 4.56 g of acetic acid (75.9 mmol) and 7.68 g of triethylamine (75.9 mmol) in a little methanol is added dropwise. After heating at reflux for 7 h, the solution is allowed to cool to room temperature. A light yellow precipitate is extracted by suction, washed in portions with 100 ml of ice-cold methanol and dried to constant weight. 11.37 g of a light yellow powder (79.3%) with a melting point of 178-179° C. (lit.: 182-184° C.) is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07807687B2 |
| Source dataset | uspto-grants-2010_10 |
| ORD ID | ord-7830f76f117a413b8d9c7cedb356d4ab |
| Source note | uspto-grants-2010_10 |