Reacción #2281980

ord-0e9d719902e241899b1fc247c6c33709

Disolventes

Condiciones de reacción

Temperatura
90°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Lavadoby washing with brine
  2. 2
    ConcentraciónThe organic layer was concentrated
  3. 3
    Otropurified (silica gel, 0-50% EtOAC/hexane)

Procedimiento

In a 100 mL round bottom flask, 1-bromo-3-methoxy-5-methyl-benzene (2.17 g, 10.79 mmol), Zn(CN)2 (1.9 g, 16.19 mmol, 1.5 eq.) and Pd(PPh3)4 (1.24 g, 1.08 mmol, 0.1 eq.) was charged with DMF (20 mL). The reaction mixture was heated at 90° C. under Ar for 7 hours. Ethyl acetate was added, followed by washing with brine. The organic layer was concentrated and purified (silica gel, 0-50% EtOAC/hexane) to give a white solid (1.31 g, 83%). 1H NMR (300 MHz, CDCl3): δ 7.05 (s, 1H), 6.97 (s, 2H), 3.81 (s, 3H), 2.39 (s, 3H).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08334295B2uspto-grants-2012_12