HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 19607917, compound → HCID 10692311, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 19607917 | HCID 19607917 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 10692311 | HCID 10692311 | 57.5% |
Reaction Steps
5-Azido-1-[4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.63 g) is dissolved in ethanol and thereto is added 10% Pd-C (0.1 g). The mixture is subjected to catalytic hydrogenation at room temperature under 1 atm. of hydrogen. Pd-C is removed by filtration and the filtrate is evaporated. The resulting residue is purified by silica gel column chromatography (eluent; dichloromethane:methanol=50:1), and recrystallized from diethyl ether to give 5-amino-1-[4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.34 g) as white powder, m.p. 198.5°-199.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05559230 |
| Source dataset | uspto-grants-1996_09 |
| ORD ID | ord-c370886228364389b7fbd063a929bffb |
| Source note | uspto-grants-1996_09 |