HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 12881937, compound → 11,12-Dihydro-4-methoxydibenz(b,f)(1,4)oxazepine-8-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 12881937 | HCID 12881937 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 11,12-Dihydro-4-methoxydibenz(b,f)(1,4)oxazepine-8-carboxylate | HCID 339237 | 77% |
Reaction Steps
A solution of ethyl 4-(2-formyl-6-methoxyphenoxy)-3-nitrobenzoate (145 g) in dioxane (1.2 l) and ethanol (150 ml) was hydrogenated over Raney nickel catalyst (60 ml) at room temperature under atmospheric pressure. After a pre-calculated amount of hydrogen was absorbed, the catalyst was removed by filtration and the filtrate was evaporated under reduced pressure. The residue was treated with ethanol (20 ml) to crystallize and then the separated crystals were collected by filtration. Recrystallization from ethanol gave ethyl 10,11-dihydro-4-methoxydibenz[b,f][1,4]oxazepine-8-caboxylate (96 g) as colorless needles. (Yield: 77%, m.p. 121°-122° C.)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04290953 |
| Source dataset | uspto-grants-1981_09 |
| ORD ID | ord-5b7da9b2a81a4b3c97052baa8800d72c |
| Source note | uspto-grants-1981_09 |