HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium sulfide nonahydrate → HCID 86732835, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium sulfide nonahydrate | HCID 73972 | — |
| Reactant | HCID 86732834 | HCID 86732834 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86732835 | HCID 86732835 | 98% |
Reaction Steps
Under N2, 1-cyclopropyl-6,7-dimethoxy-5-nitro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (10 g, 29.9 mmol) was treated with sodium sulfide nonahydrate (71.9 g, 299 mmol) in a mixture of Ethanol (100 mL) and Water (100 mL) for 2 h at 100° C. LCMS showed completion of reaction. After cooling down, the mixture was poured into cold water and the solution was adjusted to pH 2. The yellow precipitate was collected by filtration, washed with water and dried to afford 5-amino-1-cyclopropyl-6,7-dimethoxy-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (8.9 g, 29.2 mmol, 98% yield) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09340556B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-4fca75c63c4c4f38b713c79097a33e3b |
| Source note | uspto-grants-2016_05 |