반응 #509911

ord-09284f88aab742e88c2434e105699814

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척The reaction mixture was washed (H2O, 2 M aq HCl (2×), H2O, brine)
  2. 2
    건조dried (Na2SO4)
  3. 3
    농축concentrated under reduced pressure

실험 절차

To a solution of 2-amino-4-chlorobenzonitrile (7.25 g, 47.5 mmol), in anh. pyridine (38 mL, 475 mmol) and DCM (300 mL) cooled in an ice-H2O bath under Ar was added PhCOCl (5.8 mL, 50 mmol) dropwise. The reaction was allowed to slowly warm to rt within the cooling bath and then was stirred at rt overnight. The reaction mixture was washed (H2O, 2 M aq HCl (2×), H2O, brine), dried (Na2SO4) and concentrated under reduced pressure to afford the title compound as a white solid; MS (ES+): m/z 257.1 (100) [MH+]; HPLC: tR=3.27 min (OpenLynx, polar—5 min).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08101613B2uspto-grants-2012_01