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 | 4-Amino-1-Boc-piperidine | HCID 1268291 | — |
| Reactant | 4-Chloro-9-(2-trimethylsilanyl-ethoxymethyl)-9H-dipyrido[2,3-b;4',3'-d]pyrrole-6-carbonitrile | HCID 58266668 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 58266299 | HCID 58266299 | 60% |
Reaction Steps
A mixture of 4-chloro-9-(2-trimethylsilanylethoxymethyl)-9H-dipyrido[2,3-b;4′,3′-d]pyrrole-6-carbonitrile with 4-chloro-9-(2-trimethylsilanylethoxymethyl)-9H-dipyrido[2,3-b;4′,3′-d]pyrrole-6-carbonitrile (6.5:1, 85 mg, 0.24 mmol), tert-butyl 4-aminopiperidine-1-carboxylate (240 mg, 1.2 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (20 mg, 0.04 mmol), tris(dibenzylideneacetone)dipalladium(0) (16 mg, 0.02 mmol), and cesium carbonate (150 mg, 0.47 mmol) in 1,4-dioxane (2 mL) was sealed and heated at 110° C. for 2 h. The mixture was diluted with water (20 mL) and ethyl acetate (50 mL). The organic layer was separated, dried over sodium sulfate, filtered, concentrated in vacuo, and purified flash chromatography (silica, 40 g, ISCO, 5-75% ethyl acetate in heptane) to afford the title compound as a yellow solid (80 mg, 60%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09216980B2 |
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| Source dataset | uspto-grants-2015_12 |
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| ORD ID | ord-9bb48f5ea6384b2c9277df8459ffae90 |
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| Source note | uspto-grants-2015_12 |
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