HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → 4-Chloro-3-(3-fluorophenyl)-1-[2-(4-methylpiperazin-1-yl)ethyl]-5-phenyl-pyrazolo[3,4-c]pyridazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | 1-(2-Hydroxyethyl)-4-methylpiperazine | HCID 231184 | — |
| Reactant | CID 86717314 | HCID 86717314 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 4-Chloro-3-(3-fluorophenyl)-1-[2-(4-methylpiperazin-1-yl)ethyl]-5-phenyl-pyrazolo[3,4-c]pyridazine | HCID 73776179 | — |
Reaction Steps
A mixture of 4-chloro-3-(3-fluorophenyl)-5-phenyl-1H-pyrazolo[3,4-c]pyridazine (0.33 mmol), 2-(4-methylpiperazin-1-yl)ethanol (0.65 mmol), diethyl azodicarboxylate (114 mg, 0.65 mmol) and triphenyl phosphine (171 mg, 0.65 mmol) in 1,4-dioxane (2 mL) was heated using microwave irradiation to a temperature between 85 and 120° C. for a 30 to 90 min period. The reaction mixture was concentrated in vacuo and the residue was purified by preparative HPLC to provide Compound 8.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08765762B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-a9283725f954492baf72b2558935d9db |
| Source note | uspto-grants-2014_07 |