HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine, hydrochloride → 7-Methoxy-N,N-dimethyl-2-oxo-1,2,3,4-tetrahydro-3-quinolinecarboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine, hydrochloride | HCID 10473 | — |
| Reactant | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 7-Methoxy-2-oxo-1,2,3,4-tetrahydro-3-quinolinecarboxylic acid | HCID 22998619 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | 7-Methoxy-N,N-dimethyl-2-oxo-1,2,3,4-tetrahydro-3-quinolinecarboxamide | HCID 22998635 | 38.8% |
Reaction Steps
To a solution of 1,2,3,4-tetrahydro-7-methoxy-2-oxo-3-quinolinecarboxylic acid (3.74 g), dimethylamine hydrochloride (3.44 g), 1-hydroxybenzotriazole (2.85 g), and triethylamine (8.5 g) in acetonitrile (400 ml) was added WSC (6.5 g). The reaction mixture was stirred at room temperature for 24 hr and concentrated. The residue was diluted with ethyl acetate and the organic layer was washed with 1 N aqueous hydrochloric acid, 10% aqueous potassium carbonate, and saturated aqueous sodium chloride, dried, and concentrated. The resulting crude crystals were recrystallized from ethyl acetate-hexane to obtain the titled compound (1.63 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07256204B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-d431fa6599a547a981b0f99224e0fc42 |
| Source note | uspto-grants-2007_08 |