Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Binap, (A+-)- | HCID 634876 | — |
| Reactant | 4-Amino-2-methylpyridine | HCID 728670 | — |
| Reactant | HCID 21104340 | HCID 21104340 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 58866036 | HCID 58866036 | — |
Reaction Steps
4-Chloro-2-(5-chloro-2-fluoro-phenyl)-pyrrolo[2,1-f][1,2,4]triazine (30 mg, 0.106 mmole), cesium carbonate (48.5 mg, 0.149 mmole), palladium (II) acetate (1.19 mg, 0.0053 mmole), BINAP (4.96 mg, 0.0080 mmole), and 4-amino-picoline (13.8 mg, 0.128 mmole) were combined in 4 ml dioxane (anh.) and heated to 90° C. with stirring overnight. The reaction mixture was filtered to remove solid material, the filtrate was evaporated to dryness, the residue was dissolved in chloroform (8 ml), washed with 0.5 M sodium hydroxide (1 ml), dried over sodium sulfate (anh.), evaporated to dryness, and then the residue was redissolved in dimethylformamide and purified by reversed phase HPLC. The product was isolated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07977342B2 |
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| Source dataset | uspto-grants-2011_07 |
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| ORD ID | ord-67c3091ad297458f82dd7589b572c72f |
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| Source note | uspto-grants-2011_07 |
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