HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,6-Lutidine → HCID 11150214, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | 2-Aminopyridine | HCID 10439 | — |
| Reactant | 1-(2-Chloro-acetyl)-3-ethyl-urea | HCID 2304790 | — |
| Solvent | 1,3-Dimethyl-2-imidazolidinone | HCID 6661 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 11150214 | HCID 11150214 | 6% |
Reaction Steps
A solution of aminopyridine (3) (0.73 g, 4.26 mmol), N-(chloroacetyl)-N′-ethylurea (0.84 g, 5.10 mmol) and 2,6-lutidine (0.59 mL, 5.10 mmol) in 1,3-dimethyl-2-imidazolidinone (7 mL) was warmed under nitrogen at 110° C. for 5 hours. The mixture was diluted with EtOAc and washed with water (6×), then adsorbed onto silica by removal of solvent in vacuo. Silica gel chromatography (EtOAc gradient to MeOH/EtOAc (2:23)) provided the product (0.76 mg, 6%) as a solid, mp 290-294° C. (decomposed).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07563788B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-6490bd125a8a415bb210572dbd318081 |
| Source note | uspto-grants-2009_07 |