HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → N-Cyclopropyl-4-methoxy-2,6-dimethyl-N-(2-(6-(9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecan-3-yl)pyrimidin-4-yloxy)ethyl)benzenesulfonamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | N-Cyclopropyl-N-(2-hydroxyethyl)-4-methoxy-2,6-dimethylphenylsulfonamide | HCID 43577600 | — |
| Edukt | HCID 59401695 | HCID 59401695 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | N-Cyclopropyl-4-methoxy-2,6-dimethyl-N-(2-(6-(9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecan-3-yl)pyrimidin-4-yloxy)ethyl)benzenesulfonamide | HCID 46207142 | 7% |
Reaktionsschritte
To a suspension of sodium hydride (7.28 mmol, 10 equiv.) in tetrahydrofuran (10 ml) there was added, at 0° C., N-cyclopropyl-N-(2-hydroxyethyl)-4-methoxy-2,6-dimethylphenylsulfonamide (C-10) (0.8 mmol, 1.1 equiv.), followed by 3-(6-chloro-pyrimidin-4-yl)-9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane (0.73 mmol, 1 equiv.). The reaction mixture was stirrred overnight at room temperature; water was then added and the mixture was diluted with ethyl acetate. The organic phase was extracted with water and saturated sodium chloride solution, dried (Na2SO4) and concentrated in vacuo. The crude product was purified by column chromatography (Alox-neutral). Yield: 7%. Rt=3.4 min; m/z=607.5 [MH]+
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08269000B2 |
| Quelldatensatz | uspto-grants-2012_09 |
| ORD ID | ord-fdc62f7b7c2544b5af25e2e6180443b7 |
| Quellennotiz | uspto-grants-2012_09 |