Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 6-Bromo-1-chlorophthalazine | HCID 22030424 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 68453506 | HCID 68453506 | 108.5% |
Reaction Steps
A mixture of 6-bromo-1-chlorophthalazine (Example 1, 0.1 g, 0.41 mmol), piperidine (0.081 mL, 0.82 mmol) and potassium carbonate (0.056 g, 0.41 mmol) in 5 mL acetonitrile was added to a glass microwave reaction vessel. The reaction mixture was stirred and heated in a Smith Synthesizer® microwave reactor (Personal Chemistry, Inc., Upssala, Sweden) at 180° C. for 20 min. After about 20 min., all starting material was converted to product (M+1=292, 294). The mixture was concentrated under vacuum and purified via flash chromatography (silica gel) eluting with a gradient of 2% 2 M ammonia in MeOH/DCM to 6% 2 M ammonia in MeOH/DCM to give (0.13 g) 6-bromo-1-(piperidin-1-yl)phthalazine as yellow solid. Found MS (ES+): 292, 294(M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07759337B2 |
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| Source dataset | uspto-grants-2010_07 |
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| ORD ID | ord-a7ad35ad4fab489aa8ceaaf685c791ef |
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| Source note | uspto-grants-2010_07 |
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