Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178432363 | HCID 178432363 | — |
| Product | HCID 18785595 | HCID 18785595 | — |
Reaction Steps
45 ml of phosphorus oxychloride were added to 3.35 g (0.021 mole) of 2,3-dimethyl-6,7-dihydropyrrolo[2,3-d]pyridazin-7-one and the mixture was heated under reflux for 2 hours. After completion of the reaction, the reaction mixture was slowly poured into ice-water and the aqueous mixture was neutralized with an aqueous solution of sodium hydroxide. The precipitated yellow solids were collected by filtration and washed well with water. The solids were dissolved in dichloromethane and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by column chromatography through silica gel using a 15:1 mixture of chloroform and methanol as an eluent to give 2.39 g of 7-chloro-2,3-dimethylpyrrolo[2,3-d]pyridazine as a pale yellow powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06063782 |
|---|
| Source dataset | uspto-grants-2000_05 |
|---|
| ORD ID | ord-535e88c42ad84cc0bed2c0a1ce420094 |
|---|
| Source note | uspto-grants-2000_05 |
|---|