반응 #11948

ord-f1bdec720c284c5a909cb7ee228ab562

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축the reaction solution was concentrated
  2. 2
    workup.ADDITIONMethanol was added to the residue
  3. 3
    세척the mixture was washed with hexane
  4. 4
    농축The methanol layer was concentrated
  5. 5
    기타the residue was crude-purified by silica gel column chromatography (3 g, chloroform/methanol/water=7/3/0.5)

실험 절차

A mixed solution of trifluoroacetic acid (1.4 ml), thioanisole (0.36 ml), and m-cresol (0.32 ml) was added to the compound obtained in Example 14-3 (56.2 mg). After 1.5 hours, the reaction solution was concentrated. Methanol was added to the residue and the mixture was washed with hexane. The methanol layer was concentrated and the residue was crude-purified by silica gel column chromatography (3 g, chloroform/methanol/water=7/3/0.5) to obtain the title compound (18.2 mg) as colorless syrup.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07098215B2uspto-grants-2006_08