HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylenediamine → HCID 67368936, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylenediamine | HCID 3301 | — |
| Reactant | HCID 67366612 | HCID 67366612 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 67368936 | HCID 67368936 | 85% |
Reaction Steps
To a solution of methyl 1-{2-oxo-2-[5-(trifluoromethyl)pyridin-2-yl]ethyl}-1H-pyrrole-2-carboxylate (85 mg, 0.26 mmol) in 1,4-dioxane (20 mL) was added ethane-1,2-diamine (0.65 mL, 9.7 mmol). The solution was heated at reflux. After 4 days the reaction was complete (monitored by LCMS). The mixture was then concentrated in vacuo to give an oily solid. The material was purified by flash chromatography (Biotage SP4, 12 g cartridge, gradient CH2Cl2 1 CV, 0-10% MeOH in CH2Cl2 10 CV) to give 10a-[5-(trifluoromethyl)pyridin-2-yl]-2,3,10,10a-tetrahydro-1H,5H-imidazo[1,2-a]pyrrolo[1,2-d]pyrazin-5-one (70 mg, yield: 85%). ESI-MI m/z [M+H]+ 323.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08604034B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-770147cefa2243298093775ab71a216c |
| Source note | uspto-grants-2013_12 |