Reaktion #2151238

ord-bd917dc650ec40149d8330ea22309810

Lösungsmittel

Reaktionsbedingungen

Temperatur
200°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe reaction extracted with 2×75 mL of dichloromethane
  2. 2
    Trocknendried with sodium sulfate
  3. 3
    Sonstigeevaporated

Vorschrift

400 mg (0.0018 mol, 1 eq) of 4-bromo-2-fluoro-1-nitro-benzene, 330 mg (0.0018 mol, 1 eq) of D9, 350 mg (0.0027 mol, 1.5 eq) of diisopropylethylamine, and 5 mL of dimethylformamide were combined, heated to 200° C. and held for 1 min in a microwave reactor. 80 mL of water was then added and the reaction extracted with 2×75 mL of dichloromethane. The dichloromethane layers were combined, dried with sodium sulfate, and evaporated to yield N-(5-bromo-2-nitrophenyl)-1-(tetrahydro-2H-pyran-4-yl)-4-piperidinamine which was used without further purification in the next step. MS (ESI): 385 [M+H]+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08288413B2uspto-grants-2012_10