Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Azepane | HCID 8119 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Amino-4,6-dichloropyrimidine | HCID 65522 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 31537603 | HCID 31537603 | 86.8% |
Reaction Steps
In a 25 mL sealable tube under nitrogen were combined 4,6-dichloro-2-pyrimidinamine (0.50 g, 3.05 mmol) and hexahydro-1H-azepine (0.34 mL, 3.05 mmol) in CH3OH (10 mL). Triethylamine (0.47 mL, 3.35 mmol) was added, the vial was sealed, and the reaction mixture was stirred for 5 hours at 50° C. The reaction was cooled to room temperature and concentrated. The resulting yellow solid was partitioned between EtOAc and water. The organic layer was separated, dried (MgSO4), filtered and concentrated to afford the title compound (600 mg, 82%) as a yellow solid. LC-MS (ES) m/z=227 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08697685B2 |
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| Source dataset | uspto-grants-2014_04 |
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| ORD ID | ord-9a5329a34f9746299b5abde49059f7ca |
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| Source note | uspto-grants-2014_04 |
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