반응 #795509

ord-885730bb68a144cb991ec2be0bb66ebd

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Reaction mixture
  2. 2
    세척washed with water and brine
  3. 3
    건조The organic layer was dried over Na2SO4
  4. 4
    농축concentrated in vacuo
  5. 5
    기타The crude residue was triturated with ether-pentane

실험 절차

To a solution of 2-bromo-N-(prop-2-yn-1-yl)acetamide (0.7 g, 3.98 mmol) in DCM (10 mL) added N-methyl piperazine (0.66 mL, 5.96 mmol) drop wise. Reaction mixture stirred at rt for 16 h, diluted with DCM and washed with water and brine. The organic layer was dried over Na2SO4 and concentrated in vacuo. The crude residue was triturated with ether-pentane, affording the title compound (0.38 g, 49%); LCMS: m/z=196.15 (M+1); 1H NMR (300 MHz, DMSO-d6) δ 8.06 (d, J=6.1 Hz, 1H), 3.86 (dd, J=5.9, 2.5 Hz, 2H), 3.07 (t, J=2.5 Hz, 1H), 2.91 (s, 2H), 2.47-2.25 (m, 8H), 2.15 (s, 3H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09174978B2uspto-grants-2015_11