HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonium Chloride → HCID 86654263, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonium Chloride | HCID 25517 | — |
| Edukt | Potassium 4-sulfamoylphenolate | HCID 67083060 | — |
| Edukt | Tert-butyl 4-[2-(methanesulfonyloxymethyl)pyridin-5-yl]piperidine-1-carboxylate | HCID 86654264 | — |
| Lösungsmittel | Dimethyl Sulfoxide | HCID 679 | — |
| Produkt | HCID 86654263 | HCID 86654263 | 55% |
Reaktionsschritte
To a solution of tert-butyl 4-[2-(methanesulfonyloxymethyl)pyridin-5-yl]piperidine-1-carboxylate (Example 1(3)) (24 mg, 0.065 mmol) in dimethyl sulfoxide (1 mL) was added potassium 4-sulfamoylphenolate (14 mg, 0.065 mmol). The mixture was stirred at room temperature for 3.5 hours, to which was added saturated aqueous ammonium chloride solution and extracted with chloroform. The organic layer was washed with brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/8 and chloroform/methanol=200/1→20/1) to give the title compound as a white crystal (16 mg, yield 54%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08536176B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-60c14c363c0549d4b508eebe4cf55d25 |
| Quellennotiz | uspto-grants-2013_09 |