Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | HCID 21183746 | HCID 21183746 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 15860292 | HCID 15860292 | 66.7% |
Reaction Steps
A suspension of 1 g (3 mmol) of 5-methyl-4-oxo-3-phenyl-3,5-dihydro-4H-pyridazino[4,5-b]indole-1-acetic acid and of 0.7 g (4.3 mmol) of 1,1′-carbonylbis-1H-imidazole in 200 ml of tetrahydrofuran is stirred for 2 h at 60° C. The reaction mixture is cooled to 25° C., an excess of liquefied dimethylamine in solution in tetrahydrofuran is added and the reaction mixture is stirred for 72 h at room temperature. It is concentrated under reduced pressure, 300 ml of water are added and the precipitate is collected by filtration, washed with water and with ether and recrystallized from propan-2-ol. 0.75 g (2 mmol) of solid is isolated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06262045B1 |
|---|
| Source dataset | uspto-grants-2001_07 |
|---|
| ORD ID | ord-cad343a3c9134ad1b6db7e0ef648bc12 |
|---|
| Source note | uspto-grants-2001_07 |
|---|