Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | 4-Amino-1-Boc-piperidine | HCID 1268291 | — |
| Reactant | 3-Chloro-6-(trifluoromethyl)pyridazine | HCID 28242526 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 59805854 | HCID 59805854 | 85% |
Reaction Steps
A mixture of 3-chloro-6-trifluoromethyl-pyridazine (4.4 g, 24.1 mmol) (prepared by a procedure similar to that described in Tetrahedron, 1999, 55 (52), 15067-15070), 4-amino-1-tert-butyloxycarbonylpiperidine (9.63 g, 48.1 mmol) and potassium iodide (cat.) were heated in a melt at 150° C. for 30 min. After this period, the reaction mixture was diluted with water and extracted with dichloromethane. The organic layer was separated, dried and the solvent evaporated in vacuo. The crude product was purified by chromatography (silica; 1%-4% ammonia in methanol (7 M)/dichloromethane) to give D1 (7.06 g, 85%). C15H21F3N4O2 requires 346; Found 347 (MH+)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08940743B2 |
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| Source dataset | uspto-grants-2015_01 |
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| ORD ID | ord-71b79922ffd1499da15b5f34a39a8db3 |
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| Source note | uspto-grants-2015_01 |
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