HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 59708490, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Benzonitrile, 4-bromo- | HCID 12162 | — |
| Reactant | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| Reactant | HCID 59708391 | HCID 59708391 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Product | HCID 59708490 | HCID 59708490 | 36% |
Reaction Steps
Under an argon atmosphere 315 mg (3-fluoro-phenyl)-(5-oxo-2-piperazin-1-yl-6,7-dihydro-5H-5λ4-thieno[3,2-d]pyrimidin-4-yl)-amine, 165 mg 4-bromo-benzonitrile, 21 mg palladium(II)acetate, 80 mg Xantphos and 415 mg caesium carbonate are stirred in 2.50 ml degassed toluene for 24 hours at 80° C. After cooling the reaction mixture is extracted with ethyl acetate and saturated sodium chloride solution. The organic phase is dried and evaporated to dryness. The residue is purified by preparative HPLC (method A). 146 mg of the product (36%) are obtained. HPLC (method A):RT=3.83 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08604039B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-e1bb7253f508416c8f0bdfe9cee3d0fa |
| Source note | uspto-grants-2013_12 |