HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Piperidinecarboxamide → HCID 68453488, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Piperidinecarboxamide | HCID 3772 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 6-Bromo-1-chlorophthalazine | HCID 22030424 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 68453488 | HCID 68453488 | 92.7% |
Reaction Steps
A mixture of the isonipecotamide (71 mg, 554 μmol), 6-bromo-1-chlorophthalazine (Example 1, 90 mg, 370 μmol) and potassium carbonate (51 mg, 370 μmol) in 5 mL acetonitrile was added to a glass microwave reaction vessel. The reaction mixture was stirred and heated in a Smith Synthesizes microwave reactor (Personal Chemistry, Inc., Upssala, Sweden) at 190° C. for about 20 min. at which the starting material was consumed, by TLC, to form product (M+1=335, 337). The mixture was concentrated and purified by column, eluting with a gradient of 2% 2M ammonia in MeOH/DCM to 10% 2M ammonia in MeOH/DCM to give 1-(6-bromophthalazin-1-yl)piperidine-4-carboxamide (0.115g) as a pale yellow solid. Found MS (ES+): 335, 337(M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07759337B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-ac120d0c021f4a90aead0c422a009fda |
| Source note | uspto-grants-2010_07 |