반응 #1361590

ord-10f48641c6c540a9b6230d621781f096

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    기타to be consumed by TLC
  3. 3
    기타The spent catalyst was removed by filtration through a Celite pad
  4. 4
    세척the pad carefully washed with more ethanol
  5. 5
    기타The combined filtrates were evaporated in vacuo
  6. 6
    기타the residue purified by flash chromatography on silica gel (ethyl acetate

실험 절차

4-(7-chloroquinolin-4-yl)butyn-1-ol (1 g) was dissolved in ethanol (25 mL) in a Parr hydrogenation bottle and platinum (IV) oxide [Adams' Catalyst] (100 mg) was added. The Parr bottle was placed on a Parr hydrogenation apparatus and the solution hydrogenated at 50 psi for 2 hours after which time the starting material had been judged to be consumed by TLC. The spent catalyst was removed by filtration through a Celite pad and the pad carefully washed with more ethanol. The combined filtrates were evaporated in vacuo and the residue purified by flash chromatography on silica gel (ethyl acetate; then ethyl acetate:methanol, 95:5) to give the title compound (500 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06156767uspto-grants-2000_12