HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Phosphate, Tribasic → HCID 71252555, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | n,n-Dimethylpiperazine-1-carboxamide | HCID 712909 | — |
| Reactant | 2-(Dicyclohexylphosphino)biphenyl | HCID 2734216 | — |
| Reactant | [4-(3,5-Dimethylpyridin-2-yl)piperazin-1-yl](4-iodophenyl)methanone | HCID 58484535 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 71252555 | HCID 71252555 | 20.1% |
Reaction Steps
To a mixture of [4-(3,5-dimethylpyridin-2-yl)piperazin-1-yl](4-iodophenyl)methanone (270 mg) described in Preparation Example 113, palladium acetate (8 mg), 2-(dicyclohexylphosphino)biphenyl (22 mg), tripotassium phosphate (190 mg) and piperazine-1-carboxylic acid dimethylamide (111 mg) was added 1,2-dimethoxyethane (5 mL), and the mixture was stirred with heating under reflux for 7 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and the solvent was evaporated. The obtained residue was purified by NH coated silica gel column chromatography (ethyl acetate:hexane) to give the title compound (58 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08816079B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-d95a029a48b14e6484523c25214ce8a2 |
| Source note | uspto-grants-2014_08 |