Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 4-Piperidinol, 1-methyl- | HCID 66048 | — |
| Reactant | Potassium bis(trimethylsilyl)amide | HCID 3251421 | — |
| Reactant | HCID 43524568 | HCID 43524568 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 117892068 | HCID 117892068 | — |
Reaction Steps
6-chloro-3-nitro-N-[1-(pyridin-2-yl)ethyl]pyridin-2-amine E-3.8″(2 g; 7.17 mmol) is suspended in 20 ml THF and a potassium bis(trimethylsilyl)amide solution in THF (29 ml; 29 mmol) is slowly added at 25° C. After 15 min 4-hydroxy-N-methylpiperidine (3.37 g; 28.71 mmol) is added and the reaction mixture is stirred for 16 h at 25° C. The reaction mixture is diluted with ethyl acetated and water. The organic phase is separated and dried using MgSO4. The crude intermediate is purified using reversed phase chromatography (prep. HPLC1). The product containing fractions are combined and freeze-dried
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09296748B2 |
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| Source dataset | uspto-grants-2016_03 |
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| ORD ID | ord-8d7eb0be73044f32a31dd6911c9fe88a |
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| Source note | uspto-grants-2016_03 |
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