Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Butanol | HCID 263 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | 3,6-Dichloropyridazine | HCID 67331 | — |
| Reactant | 1-Benzyl-4-piperidylamine | HCID 415852 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 28530649 | HCID 28530649 | 41% |
Reaction Steps
A mixture of 4-amino-1-benzylpiperidine (4 g, 21 mmol) and 3,6-dichloro-pyridazine (1.56 g, 10.5 mmol) was stirred for 1 h at 120° C., before n-butanol (10 ml) was added and the reaction mixture stirred for a further 1 h at 120° C. After addition of water and dichloromethane, the organic layer was separated, dried (Na2SO4), filtered and the solvent evaporated in vacuo. The residue was crystallized from acetonitrile and the resulting solid was filtered off and dried to yield D1 (1.3 g, 41%) as a solid. C16H19ClN4 requires 302. Found 303 (MH+); mp: 208.2-209.3° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08466153B2 |
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| Source dataset | uspto-grants-2013_06 |
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| ORD ID | ord-3e895b78de8e4e02ada4d41a0238e64c |
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| Source note | uspto-grants-2013_06 |
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