HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 21106537, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| Reactant | 1-tert-Butyl-3-methyl-1H-pyrazol-5-amine | HCID 737200 | — |
| Reactant | HCID 21106551 | HCID 21106551 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 21106537 | HCID 21106537 | — |
Reaction Steps
200 mg 4-Bromo-2-(4-chloro-phenyl)-2H-phthalazin-1-one (prepared as described in Method R), 91 mg 1-tert.-butyl-3-methyl-1H-pyrazol-5-ylamine, 310 mg cesium carbonate, 21 mg 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene and 16.4 mg tris-(di-benzylideneacetone)-dipalladium in 2 ml dry dioxane were stirred under nitrogen at 100° C. for 18 hrs. The solvent was removed under vacuum and the residue stirred with 50 ml water. The crude product was isolated by filtration, washed with water and purified by chromatography on silica, eluting sequentially with heptane, DCM and finally DCM/MeOH 60:1. Yield 180 mg (74%) of the title product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07501410B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-936b886980574373bfd547f0b63a6006 |
| Source note | uspto-grants-2009_03 |