HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperidine → HCID 66955386, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | PyBroP | HCID 2733179 | — |
| Reactant | HCID 66955389 | HCID 66955389 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 66955386 | HCID 66955386 | — |
Reaction Steps
To a stirred solution of ethyl 6-methyl-2-oxo-4-p-tolyl-1,2-dihydropyrimidine-5-carboxylate (2 g; 7,34 mmol) in dioxane (35 mL) were added PyBrOP (3,77 g; 8,08 mmol), triethyl amine (2,06 mL; 14,69 mmol) and piperidine (0,945 mL; 9,55 mmol) and the mixture was stirred at room temperature for 4 days. The reaction mixture was diluted with ethyl acetate and washed with a saturated solution of ammonium chloride and brine, dried over sodium sulphate, filtered and concentrated under reduced pressure. Purification by flash-chromatography on silica gel using a gradient of ethyl acetate (2-20%) in heptane furnished 2 g (80%) of the title as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08906906B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-110bf5f969074b1290666e08e3b0ec5d |
| Source note | uspto-grants-2014_12 |