HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Chloride → HCID 23442376, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | Tributylphenyltin | HCID 607632 | — |
| Reactant | HCID 12985703 | HCID 12985703 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 23442376 | HCID 23442376 | 34.3% |
Reaction Steps
A mixture of 5-bromo-1-methyl-1,4-dihydro-9H-pyrazolo[4,3-b]quinolin-9-one (EXAMPLE 5, 50 mg, 0.18 mmol), tributylphenyltin (0.12 ml, 0.36 mmol), tetrakis(triphenylphosphine)palladium (0) (62 mg, 0.054 mmol) and lithium chloride (19 mg, 0.45 mmol) in 1,4-dioxane (2 ml) was refluxed for 16 h. After cooling to room temperature, the mixture was evaporated, dissolved in ethyl acetate (20 ml) and the insoluble material was filtered off. The filtrate was concentrated in vacuo and purified by preparative thin layer chromatography developing with ethyl acetate/hexane (1/2). The obtained solid was recrystallized from diethyl ether to afford 17 mg (33%) of the title compound as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06686373B2 |
| Source dataset | uspto-grants-2004_02 |
| ORD ID | ord-dc5ca70dbfca4a3b85490f954869954a |
| Source note | uspto-grants-2004_02 |