Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyclohexylamine | HCID 7965 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 6-Bromo-1-chlorophthalazine | HCID 22030424 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 68455291 | HCID 68455291 | 68.6% |
Reaction Steps
A mixture of 6-bromo-I-chlorophthalazine (Example 1, 0.245 g, 1 mmol), cyclohexanamine (0.22 g, 2 mmol) and potassium carbonate (0.14 g, 1 mmol) in 5 mL acetonitrile were 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 20 min., all starting material was converted to product (M+1=306, 308). 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 (0.21 g) 6-bromo-N-cyclohexylphthalazin-1-amine as a yellow solid. Found MS (ES+): 306, 308(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-73a12226d95147919e8e7e90095aac0b |
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| Source note | uspto-grants-2010_07 |
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