HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 15485021, compound → HCID 15485025, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 15485021 | HCID 15485021 | — |
| Catalyst | Palladiumcarbon | HCID 14818447 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 15485025 | HCID 15485025 | 40.8% |
Reaction Steps
1-Bromo-2,4,5,6-tetrafluoro-3-[(4-methoxyphenyl)aminosulfonyl]benzene (250 mg, 0.6 mmol) (Example 5) was dissolved in methanol (25 ml) and placed in a closed vessel. A catalytic amount of 10% Pd/charcoal (25 mg) was added and the mixture was hydrogenated at 60 psi H2 for 4 h. The mixture was filtered through celite, the solvent was evaporated and the residue was purified by chromatography (silica; EtOAc/Hexane, 1:4) to yield 82 mg of the title compound. 1H-NMR (CDCl3): δ 7.10 (2H, dd, J=9.0 and 2.0 Hz), 6.94 (1H, br s), 6.85 (1H, m). 6.79 (2H, dd, J=9.0 and 2.0 Hz), 3.75 (3H, s). MS(EI): 335 (20, M+), 122 (100). Anal. Calcd. for C13H9F4NO3S: C, 46.57; H, 2.71; N, 4.18; S, 9.56. Found: C, 46.46; H, 2.67; N, 4.17; S, 9.52.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06284923B1 |
| Source dataset | uspto-grants-2001_09 |
| ORD ID | ord-d80d5d9207bf44beafa9b4189412675f |
| Source note | uspto-grants-2001_09 |