HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 57812854, compound → HCID 57812829, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 57812854 | HCID 57812854 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 57812829 | HCID 57812829 | 48.6% |
Reaction Steps
7 g of 4-fluoro-2-nitro-5-perhydro-1,4-oxazepin-4-ylphenylamine in solution in 170 mL of methanol are hydrogenated under 1 bar of hydrogen pressure in the presence of 700 mg of palladium-on-charcoal at 22° C. for 10 hours. The reaction crude is filtered through celite and the filtrate is concentrated under vacuum in a rotary evaporator. After evaporation, the reaction crude is purified by flash chromatography (elution dichloromethane/methanol). 3 g of 4-fluoro-5-perhydro-1,4-oxazepin-4-ylbenzene-1,2-diamine are isolated. 1H NMR spectrum (400 MHz, DMSO-d6, δ in ppm): 1.88 (m, 2H); 3.11 (m, 4H); from 3.64 to 3.74 (m, 4H); 4.20 (broad s, 2H); 4.26 (broad s, 2H); from 6.25 to 6.31 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09126969B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-1d9e609a982d4a17b5eafa54726e6748 |
| Source note | uspto-grants-2015_09 |