HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Amino-5,5-dimethyl-2-cyclohexen-1-one → 9-(4-fluoro-3-chlorophenyl)-3,4,6,7,9,10-hexahydro-3,3,6,6-tetramethyl-1,8(2H,5H)-acridinedione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Amino-5,5-dimethyl-2-cyclohexen-1-one | HCID 136680 | — |
| Reactant | 3-Chloro-4-fluorobenzaldehyde | HCID 593866 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 9-(4-fluoro-3-chlorophenyl)-3,4,6,7,9,10-hexahydro-3,3,6,6-tetramethyl-1,8(2H,5H)-acridinedione | HCID 22117865 | 15% |
Reaction Steps
A solution of 1.39 g of 3-amino-5,5-dimethyl-2-cyclohexen-1-one and 793 mg of 4-fluoro-3-chlorobenzaldehyde in 10 ml of absolute ethanol and 1 ml of 1M aqueous hydrochloric acid was heated at reflux under a nitrogen atmosphere for 18 hours. The cooled mixture was filtered and the residue was washed with 25 ml of cold diethyl ether. Crystallization from absolute ethanol/water gave 302 mg of 9-(4-fluoro-3-chlorophenyl)-3,4,6,7,9,10-hexahydro-3,3,6,6-tetramethyl-1,8(2H,5H)-acridinedione as a pale yellow crystalline solid of melting point 274-275° C. (decomposition).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05969139 |
| Source dataset | uspto-grants-1999_10 |
| ORD ID | ord-e1a7bbf274a74e0586ef7b9fa0918056 |
| Source note | uspto-grants-1999_10 |