HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 4-(6-Bromophthalazin-1-yl)piperazin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Piperazin-2-one | HCID 231360 | — |
| Reactant | 6-Bromo-1-chlorophthalazine | HCID 22030424 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 4-(6-Bromophthalazin-1-yl)piperazin-2-one | HCID 68455278 | 83.2% |
Reaction Conditions
| Temperature | 190 °C |
|---|
Reaction Steps
A glass microwave reaction vessel was charged with 6-bromo-1-chlorophthalazine (Example 1, 0.11 g, 0.45 mmol), piperazin-2-one (0.090 g, 0.90 mmol), potassium carbonate (0.062 g, 0.45 mmol) and 5 mL acetonitrile. The reaction mixture was stirred and heated in a Smith Synthesizer® microwave reactor (Personal Chemistry, Inc., Upssala, Sweden) at 190° C. for about 12 min (watts, Powermax feature on, ramp time 1 min). The mixture was purified directly via flash chromatography (silica gel) eluting with 5% 2 M ammonia methanol/DCM to give the 4-(6-bromophthalazin-1-yl)piperazin-2-one (0.115 g) as a pale yellow solid. Found MS (ES+): 307, 309(M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07759337B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-6a374d8e9a90413799d8eea059603c92 |
| Source note | uspto-grants-2010_07 |