HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → 2-[4-Chloro-5-(3-fluorophenyl)-3-phenyl-pyrazolo[3,4-c]pyridazin-1-yl]-1-pyrrolidin-1-yl-ethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | 2-Hydroxy-1-(pyrrolidin-1-yl)ethan-1-one | HCID 6480485 | — |
| Reactant | CID 86717365 | HCID 86717365 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 2-[4-Chloro-5-(3-fluorophenyl)-3-phenyl-pyrazolo[3,4-c]pyridazin-1-yl]-1-pyrrolidin-1-yl-ethanone | HCID 73776182 | — |
Reaction Steps
A mixture of 4-chloro-5-(3-fluorophenyl)-3-phenyl-1H-pyrazolo[3,4-c]pyridazine (0.33 mmol), 2-hydroxy-1-(pyrrolidin-1-yl)ethanone (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 11.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08765762B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-0ffc2a98f2514604b72b6420b9a67ea0 |
| Source note | uspto-grants-2014_07 |