HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 86600244, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 23151247 | HCID 23151247 | — |
| Reactant | HCID 178418416 | HCID 178418416 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Catalyst | Ferrocene-1,1'-bis-(diphenylphosphine) | HCID 635956 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86600244 | HCID 86600244 | 63% |
Reaction Steps
6-bromo-3-{2-fluoroethoxy-4-[3-(1-pyrrolidinyl)propoxy]phenyl}-2-methyl-4(3H)-quinazolinone synthesized in Example 204 (37 mg), palladium(II) acetate (2 mg), dppf (1,1′-bis(diphenylphosphino)ferrocene) (8.2 mg) and triethylamine (22 mg) were mixed in ethanol (5 mL), and the atmosphere in the system was replaced by carbon monoxide. The mixture was then heated under reflux in the carbon monoxide atmosphere for 2 days. Ethyl acetate was added to the reaction liquid, and the solid precipitate was filtered off. The filtrate was concentrated, purified by silica gel thin layer chromatography (chloroform/methanol=10/1), and the title compound (23 mg, 63%) was thus obtained as a light gray solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08268842B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-4c79eca8ff9448afb2910717465125b6 |
| Source note | uspto-grants-2012_09 |