HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 21183744, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Chloromethyl Methyl Ether | HCID 7864 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 135810259 | HCID 135810259 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21183744 | HCID 21183744 | 94.5% |
Reaction Steps
A suspension of 3.9 g (11 mmol) of ethyl 8-fluoro-4-oxo-3-phenyl-3,5-dihydro-4H-pyridazino[4,5-b]indole-1-carboxylate in 200 ml of dimethylformamide is added to a suspension of 0.66 g (16 mmol) of sodium hydride in 100 ml of dimethylformamide. The mixture is stirred for 1.5 h at room temperature and a solution of 1.15 ml (14.3 mmol) of chloromethoxymethane in 10 ml of tetrahydrofuran is added. The mixture is stirred for 2 h, a solution of dilute hydrochloric acid is added and the precipitate is collected by filtration and dried under reduced pressure. 4.1 g (10.4 mmol) of solid are isolated, which solid is used as is in the following stage.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06262045B1 |
| Source dataset | uspto-grants-2001_07 |
| ORD ID | ord-68417b067fb24e0b93f4a857c53bed93 |
| Source note | uspto-grants-2001_07 |