HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → N,N-diisobutyl-4-({3-[methyl(2-pyridin-2-ylethyl)amino]propyl}amino)-3-nitrobenzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | N~1~-[2-(Pyridin-2-yl)ethyl]propane-1,3-diamine | HCID 20192832 | — |
| Reactant | 4-fluoro-N,N-diisobutyl-3-nitrobenzamide | HCID 60749158 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | N,N-diisobutyl-4-({3-[methyl(2-pyridin-2-ylethyl)amino]propyl}amino)-3-nitrobenzamide | HCID 69029055 | 92% |
Reaction Steps
A mixture of 4-fluoro-N,N-diisobutyl-3-nitrobenzamide (2.07 g, 1 eq), N-(2-pyridin-2-ylethyl)propane-1,3-diamine (1.6 g, 1.2 eq) and cesium carbonate (4.5 g, 2 eq) in acetonitrile (70 ml) is heated under reflux for 3 hours then concentrated under reduced pressure at 40° C. The residue is taken up in dichloromethane (100 ml) and water (40 ml). After decantation and extraction, the combined organic phases are washed with salt water, dried over Na2SO4 then evaporated under reduced pressure at 40° C. Purification of the residue by flash chromatography on silica gel (eluent: dichloromethane 100 to dichloromethane/methanol 8:2) produces the expected compound in the form of a yellow oil (3.1 g; 92% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08236965B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-7cba77d113594c7b963578ca3eb170d1 |
| Source note | uspto-grants-2012_08 |