반응 #49089

ord-e9b1ab97345d4dc9918fcfef0393f96d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출After 6 days the reaction mixture was extracted with ethyl acetate
  2. 2
    세척washed with sodium bicarbonate solution
  3. 3
    건조dried (Na2SO4)
  4. 4
    기타evaporated in vacuo

실험 절차

To an ice-cooled suspension of dibenzylamine hydrochloride (13.5 g; 0.058 mol) and cyclopentanone (4.86 g; 0.058 mol) in 25% ethanol in water (100 ml) was added ethanol (60 ml) and a solution of potassium cyanide (3.78 g; 0.058 mol) in water (35 ml) dropwise over 20 minutes with stirring. After 6 days the reaction mixture was extracted with ethyl acetate, washed with sodium bicarbonate solution, dried (Na2SO4) and evaporated in vacuo to afford the title compound as an off white solid (8.32 g, 49%). 1H NMR (CDCl3) δ: 1.72 (6H, m), 2.12 (2H, m), 3.78 (4H, m), 7.1-7.3 (10H, m); Mass Spectrum (Electrospray LC/MS): Found 264 (MH+−HCN). C20H22N2 requires 290. Ret. time 1.88 min.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07745642B2uspto-grants-2010_06