HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Iodo-4-nitrobenzene → HCID 22181611, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Iodo-4-nitrobenzene | HCID 12495 | — |
| Reactant | 1,2-Diaminocyclohexane, trans- | HCID 43806 | — |
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | 2-Hydroxy-3-methylpyridine | HCID 70481 | — |
| Catalyst | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 22181611 | HCID 22181611 | 36% |
Reaction Steps
1-Iodo-4-nitrobenzene (1.61 g, 6.45 mmol) was combined with 3-methyl-2-pyridone (0.845 g, 7.74 mmol), CuI (0.246 g, 1.29 mmol), and K3PO4 (2.74 g, 12.9 mmol). 1,4-Dioxane (6 mL) was added followed by trans-1,2-diaminocyclohexane (0.194 mL, 1.61 mmol). The mixture was heated to reflux for 19 h before cooling and diluting with EtOAc. The mixture was filtered through a plug of silica, eluting with EtOAc, and the filtrate concentrated under reduced pressure. Purification of the crude product by flash chromatography provided 159-a (0.528 g, 36%) as a brown solid. MS: APCI (AP+): 231.1 (M)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07407974B2 |
| Source dataset | uspto-grants-2008_08 |
| ORD ID | ord-6392b6cba8d54e6d877be258a718e356 |
| Source note | uspto-grants-2008_08 |