HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide → 4-((1-(1,3-Difluoropropan-2-yl)-4-fluoropiperidin-4-yl)methoxy)-3-nitrobenzenesulfonamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | 1,3-Difluoroacetone | HCID 228397 | — |
| Edukt | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Edukt | 4((4-Fluoropiperidin-4-yl)methoxy)-3-nitrobenzenesulfonamide | HCID 67126502 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 4-((1-(1,3-Difluoropropan-2-yl)-4-fluoropiperidin-4-yl)methoxy)-3-nitrobenzenesulfonamide | HCID 67422931 | — |
Reaktionsschritte
To a suspension of EXAMPLE 341C (0.100 g) and 1,3-difluoropropan-2-one (0.025 g) in dichloromethane (2 mL) was added sodium triacetoxyborohydride (0.071 g). After 15 minutes, N,N-dimethylformamide was added dropwise until an orange solution resulted (−15 drops). After stirring overnight additional 1,3-difluoropropan-2-one and sodium triacetoxyborohydride were added. After 3 hours, the reaction was loaded onto silica gel (Reveleris 40 g) and eluted with a gradient of 0.5-5% methanol/dichloromethane over 30 minutes (flow=40 ml/minutes) to provide the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09029404B2 |
| Quelldatensatz | uspto-grants-2015_05 |
| ORD ID | ord-16aaffaa1c0345aea03d2c6139ed2bc1 |
| Quellennotiz | uspto-grants-2015_05 |