HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Aminoacetophenone → HCID 11572724, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Aminoacetophenone | HCID 7468 | — |
| Reactant | 1,3-Bis(diphenylphosphino)propane | HCID 81219 | — |
| Reactant | 2,6-Dichloro-4-iodopyridine | HCID 11737393 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 11572724 | HCID 11572724 | — |
Reaction Steps
To 2,6-dichloro-4-iodopyridine (0.8177 g, 3 mmol) and 4-aminoacetophenone (0.4891 g, 3.6 mmol) dissolved in dry toluene (10 mL) and THF (2 mL) was added tris(dibenzylideneacetone)dipalladium(0) (0.0571 g, 0.06 mmol), 1,3-bis(diphenyl-phospino)propane (0.0499 g, 0.12 mmol), and sodium-tert-butoxide (0.4042 g, 4.2 mmol). The reaction mixture was stirred and refluxed for 12 to 14 hours under N2. The reaction mixture was diluted with CH2Cl2 and filtered through Celite™, then rinsed with CH2Cl2. The filtrate was washed two times with water and one time with brine. The organic phase was collected and dried over potassium carbonate. The filtered sample was concentrated, and the resulting solid was dried for 12-18 hours under vacuum.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07622486B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-33bd660ad50f493295d2bad1d61534bf |
| Source note | uspto-grants-2009_11 |