Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Thiomorpholine | HCID 67164 | — |
| Edukt | 1-(5-Chloro-2-nitrophenyl)piperidine | HCID 3096079 | — |
| Produkt | 4-(4-Nitro-3-piperidin-1-ylphenyl)morpholine | HCID 4373472 | 66% |
Reaktionsschritte
A mixture of 172 mg (0.715 mmol) 1-(5-chloro-2-nitro-phenyl)-piperidine (as prepared in Example 4, step (a)) and 360 μL (3.58 mmol) of thiomorpholine were heated with stirring under Ar at 140° C. for 40 h. After cooling to RT, the mixture was poured into water (50 mL) and extracted with EtOAc (2×20 mL). The combined extracts were washed with water (3×50 mL) and brine (50 mL) and then dried (Na2SO4). Concentration and chromatography on a 10-g silica SPE column with 60% dichloromethane-hexane afforded 145 mg (66%) of the title compound as a yellow resin: Mass spectrum (ESI, m/z): Calcd. for C15H21N3O2S, 308.1 (M+H), found 308.1.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07705042B2 |
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| Quelldatensatz | uspto-grants-2010_04 |
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| ORD ID | ord-f3b5db19c1274465b5cb652ebac8fd66 |
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| Quellennotiz | uspto-grants-2010_04 |
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