HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 58118746, compound → HCID 58118798, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 58118746 | HCID 58118746 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 58118798 | HCID 58118798 | 17.5% |
Reaction Steps
To a mixture of 2-fluoro-6-nitro-3-pyrrolidin-1-ylaniline (285 mg, 1.26 mmol) in ethanol (20 ml) was added a slurry of Raney nickel (approximately 100 mg) in ethanol. The mixture was stirred under a hydrogen atmosphere (1 atm) at rt overnight. The reaction was purged of hydrogen, flushed with nitrogen and then filtered through a pad of Celite® using ethanol to rinse. The filtrate was concentrated under reduced pressure to afford crude product (43 mg, 17%) which was used without purification. 1H NMR (300 MHz, DMSO-d6) 6.19 (dd, J=8.4, 1.5 Hz, 1H), 5.89 (dd, J=8.4, 8.4 Hz, 1H), 4.30 (s, 2H), 4.20 (s, 2H), 2.94-3.07 (m, 4H), 1.72-1.89 (m, 4H); ES-MS m/z 196.3 (MH)+; HPLC RT (Method B) 1.08 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08338594B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-33f2801c0651400aa4dcc0fdd51372e1 |
| Source note | uspto-grants-2012_12 |