반응 #83378

ord-3cc22d280f9e419d99ac593603a5640b

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed with a saturated aqueous sodium hydrogen carbonate, water, 1N-hydrochloric acid, water
  2. 2
    건조a saturated aqueous sodium hydrogen carbonate, water and an aqueous sodium chloride, successively, and then dried
  3. 3
    농축The resulting solution was concentrated under reduced pressure
  4. 4
    기타the residue was purified on silica gel column chromatography

실험 절차

To a solution of the FR-900506 substance (30.5 mg) in pyridine (1 ml) was added p-nitrobenzoyl chloride (ca. 100 mg), and the mixture was stirred at room temperature for 2 hours. The reaction mixture was diluted with ethyl acetate, and washed with a saturated aqueous sodium hydrogen carbonate, water, 1N-hydrochloric acid, water, a saturated aqueous sodium hydrogen carbonate, water and an aqueous sodium chloride, successively, and then dried. The resulting solution was concentrated under reduced pressure, and the residue was purified on silica gel column chromatography to give 17-allyl-1,14-dihydroxy-23,25-dimethoxy-13,19,21,27-tetramethyl-12-[2-[4-(p-nitrobenzoyloxy)-3-methoxycyclohexyl]-1-methylvinyl]-11,28-dioxa-4-azatricylco[22.3.1.04,9 ]octacos-18-ene-2,3,10,16-tetraone (37.7 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05624842uspto-grants-1997_04