HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyclohexylamine → 6-Fluoro 4-hydroxy-1-methyl-2-oxo-1,2-dihydro-quinoline-3-carboxylic acid cyclohexylamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyclohexylamine | HCID 7965 | — |
| Reactant | 3-Quinolinecarboxylic acid,6-fluoro-1,2-dihydro-4-hydroxy-1-methyl-2-oxo-,ethyl ester | HCID 69477250 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 6-Fluoro 4-hydroxy-1-methyl-2-oxo-1,2-dihydro-quinoline-3-carboxylic acid cyclohexylamide | HCID 69475565 | 97% |
Reaction Steps
Cyclohexylamine (1.98 mL, 17.34 mmol) was added to a solution of Compound 41 (2.3 g, 8.67 mmol) in toluene (50 mL) and refluxed for 4 h. The solution was cooled and the solvent was evaporated under vacuum. The residue obtained was suspended in water, briefly sonicated, and filtered. The crude product was recrystallized by ether to yield 2.38 g (97%) of white solids. M.P. 193° C. 1H NMR (DMSO-d6): δ 1.28 (m, 1H), 1.36 (m, 4H), 1.55 (m, 1H), 1.68 (m, 2H), 1.87 (m, 2H), 3.62 (s, 3H), 3.90 (m, 1H), 7.70 (m, 3H), 7.77 (d, J=8.0 Hz, 1H), 10.41 (s, 1H). EIMS m/z 341 (M+23).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07312221B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-f29099edc047483195ee52e026d0c611 |
| Source note | uspto-grants-2007_12 |