Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 87170685 | HCID 87170685 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 66825611 | HCID 66825611 | 99% |
Reaction Steps
NH4Cl (0.15 g, 2.79 mmol) was added to a stirred solution of rac-4-(3-bromo-phenyl)-4-methyl-4,5-dihydro-pyrazolo[1,5-a]pyrazine-6-thione (0.45 g, 1.40 mmol) in EtOH (50 mL) and the mixture was heated at 80° C. for 28 hours. The solvent was removed in vacuo and the residue was dissolved in DCM and washed with water. The organic layer was separated, dried (MgSO4), filtered and the solvents evaporated in vacuo. The crude product was purified by flash column chromatography (silica gel; 7 M solution of ammonia in methanol in AcOEt 0/100 to 20/80). The desired fractions were collected and concentrated in vacuo to yield rac-4-(3-bromo-phenyl)-4-methyl-4,7-dihydro-pyrazolo[1,5-a]pyrazin-6-ylamine (0.42 g, 99% yield) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08609660B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-c608e0fda4d747cbb8b7b8be08c42c9f |
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| Source note | uspto-grants-2013_12 |
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