HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86725454, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | HCID 86725452 | HCID 86725452 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86725454 | HCID 86725454 | 82.6% |
Reaction Steps
A solution of piperazine (45.2 g, 525 mmol) in ethanol (300 mL) was heated to reflux. A solution of 2-tert-butyl-4-chloro-6-(2-methoxy-ethyl)-pyrimidine (20 g, 87 mmol) in ethanol (50 mL) was added dropwise to the above solution. The solution was refluxed for another 3 hrs, cooled to room temperature. Then water was added and the organic layer was extracted with EA (400 mL×3). To the organic layer was added 5% citric acid (1 L), separated, and the aqueous layer was collected and adjusted to alkaline pH>8 with 2 N NaOH. The alkaline aqueous layer was extracted with EA (400 mL×3), and the organic phase was dried over Na2SO4, filtered and concentrated to give the title compound (20 g, 82% yield) as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09376396B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-5f065abd1c9a47408506deb5f8e6574b |
| Source note | uspto-grants-2016_06 |