Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 4-(Diphenylmethoxy)-1-piperidinepropaneamine | HCID 10969393 | — |
| Reactant | HCID 57099090 | HCID 57099090 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 53956986 | HCID 53956986 | 38.8% |
Reaction Steps
563 mg of 4-(diphenylmethoxy)-1-piperidinepropanamine and 442 mg of tert-butyl (6-chloro[1,2,4]triazolo[1,5-b]pyridazin-2-yl)carboxylate were dissolved in 5 ml of pyridine, followed by stirring at 80° C. for 13.5 hours. After cooling, water was added, followed by extraction with ethyl acetate; the extract was washed with saturated saline and dried with magnesium sulfate. The dry product was concentrated under reduced pressure; the residue was subjected to silica gel column chromatography and eluted with ethyl acetate:methanol:triethylamine (50:5:1). The desired fraction was collected and concentrated under reduced pressure; the residue was crystallized by the addition of ethyl acetate, collected by filtration, washed with ethyl ether and dried to yield 365 mg of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06248740B1 |
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| Source dataset | uspto-grants-2001_06 |
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| ORD ID | ord-3c1a9b9965054197904665b51c59a189 |
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| Source note | uspto-grants-2001_06 |
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