HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl sulfate(1-) → 52793-97-2
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl sulfate(1-) | HCID 4694097 | — |
| Reactant | 3-[[4-(Dimethylamino)phenyl]methylene]-1,7,7-trimethylbicyclo[2.2.1]heptan-2-one | HCID 68125345 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 52793-97-2 | HCID 20981548 | 140.7% |
Reaction Steps
750 g of 4-dimethylamino benzylidene camphor (prepared in Example 1) and 334 g of methyl sulfate are progressively heated to reflux in ethyl acetate. An exothermic precipitation suddenly occurs and when it has abated the reaction mixture is then heated for three hours at reflux. A pale yellow solid precipitates which is then filtered, washed with ethyl acetate and recrystallized in a benzene-acetonitrile mixture, yielding 866 g of white product melting at 20° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04061730 |
| Source dataset | uspto-grants-1977_12 |
| ORD ID | ord-cc72ffd0a07d4b05a11cd814e9743312 |
| Source note | uspto-grants-1977_12 |