反応 #83378

ord-3cc22d280f9e419d99ac593603a5640b

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄washed with a saturated aqueous sodium hydrogen carbonate, water, 1N-hydrochloric acid, water
  2. 2
    乾燥a saturated aqueous sodium hydrogen carbonate, water and an aqueous sodium chloride, successively, and then dried
  3. 3
    濃縮The resulting solution was concentrated under reduced pressure
  4. 4
    その他the residue was purified on silica gel column chromatography

実験手順

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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05624842uspto-grants-1997_04