HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 3-Amino-1-methyl-5-phenyl-1H-benzo[E][1,4]diazepin-2(3H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 1H-1,4-Benzodiazepine-2,3-dione, 1-methyl-5-phenyl-, 3-oxime | HCID 4293899 | — |
| Catalyst | Nickel | HCID 935 | — |
| Product | 3-Amino-1-methyl-5-phenyl-1H-benzo[E][1,4]diazepin-2(3H)-one | HCID 2729681 | 95% |
Reaction Steps
A solution of 150 ml of methanol containing 5 g (17.9 mmole) of 1,3-dihydro-1-methyl-3-oximino-5-phenyl-1,4-benzodiazepin-2-one was treated with a slurry of active Raney-nickel catalyst1 (10 g wet weight). The resulting suspension was hydrogenated on a Parr apparatus at 60 psi and 23° C. for 30 hours. The catalyst was removed by filtration and the filtrate was concentrated to afford the title compound in 95% yield. Rf =0.23 (chloroform-ethanol, 95:5), Rf =0.23 (chloroform-methanol-acetic acid-water, 90:10:1:1)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05004741 |
| Source dataset | uspto-grants-1991_04 |
| ORD ID | ord-a8152ff2468349fd81f02226e0a1271e |
| Source note | uspto-grants-1991_04 |