HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 178467253, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Dicyclohexylcarbodiimide | HCID 10868 | — |
| Reactant | 2-Dimethylaminopyridine | HCID 21885 | — |
| Reactant | 5-(2-Chlorophenyl)cyclohexane-1,3-dione | HCID 875360 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178467253 | HCID 178467253 | 78.5% |
Reaction Steps
To a solution of 5-(2-chlorophenyl)cyclohexane-1,3-dione (1.5 g), acetic acid (0.73 g) and dimethylaminopyridine (0.12 g) in dimethylformamide (65 ml) was added dicyclohexylcarbodiimide (1.5 g), and the mixture was stirred at room temperature for 13 hours. Under reduced pressure, the solvent was evaporated, and to the residue was ethyl acetate. The solution was washed with sodium hydrogen carbonate solution, water and saturated brine, dried with magnesium sulfate and concentrated under reduced pressure, and the residue was recrystallized from ethyl acetate-hexane to give colorless crystals of 2-(1-hydroxyethylidene)-5-(2-chlorophenyl)cyclohexane-1,3-dione (1.4 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06350749B1 |
| Source dataset | uspto-grants-2002_02 |
| ORD ID | ord-6fef7cff67d94b209e2caa9ada4ebe25 |
| Source note | uspto-grants-2002_02 |