HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 15958274, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | 5-bromo-N-(4-fluorobenzyl)-8-hydroxy-1,6-naphthyridine-7-carboxamide | HCID 22346401 | — |
| Solvent | 2(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl- | HCID 81646 | — |
| Product | HCID 15958274 | HCID 15958274 | — |
| Product | HCID 21903395 | HCID 21903395 | — |
Reaction Steps
To a solution of 5-bromo-N-(4-fluorobenzyl)-8-hydroxy-1,6-naphthyridine-7-carboxamide from example 126 (45 mg, 0.120 mmol), N-methylpiperazine (79.8 ul, 0.72 mmol) in DMPU (0.50 ml) was heated at 135 C for 18 hrs. The resulting mixture was treated with TFA (100 ul) and purified by preparative HPLC (Gilson Semi Preparative HPLC System and a YMC Combiprep Pro Column (50×20 mm i.d., C18, S-5 um, 120A) eluting with 5-95% acetonitrile/water (0.1%) at 15 ml/min) to afford the piperazin-4-ium trifluoroacetate salt of the title compound after lyophillization.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06921759B2 |
| Source dataset | uspto-grants-2005_07 |
| ORD ID | ord-149f74489de94eba80d117f61ea8be27 |
| Source note | uspto-grants-2005_07 |