HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperazine → HCID 66953548, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | 8-Bromo-2-methoxy-1,5-naphthyridine | HCID 53421617 | — |
| Solvent | 1-Pentanol | HCID 6276 | — |
| Product | HCID 66953548 | HCID 66953548 | 96.2% |
Reaction Steps
A solution of 8-bromo-2-methoxy-[1,5]naphthyridine (4.78 g, 20 mmol, prepared as in WO 2006/032466) and piperazine (8.6 g, 100 mmol) in 1-pentanol (20 mL) was heated at 80° C. over night. The mixture was cooled and the precipitate filtered off. The filtrate was diluted with EA (100 mL) and washed with water (20 mL). The aq. phase contains some product, which was extracted with DCM/MeOH 9:1 (3×30 mL). The org. phases were combined, dried over MgSO4 and concentrated under reduced pressure. The residue was purified by CC (EA/MeOH 4:1 to MeOH) to give the desired intermediate (4.7 g, 96%) as yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08217029B2 |
| Source dataset | uspto-grants-2012_07 |
| ORD ID | ord-de8af0105e6a443eaa43fb9f7b105f2d |
| Source note | uspto-grants-2012_07 |