反应详情

温度

100 °C

To a solution of methyl 2-((S)-6-((R)-7-fluoro-4-(4-hydroxy-2,6-dimethylphenyl)-2,3-dihydro-1H-inden-1-yloxy)-2,3-dihydrobenzofuran-3-yl)acetate (100 mg) in N,N-dimethylformamide (2 mL) is added Cs2CO3 (106 mg) and 1-oxa-6-thiaspiro[2.5]octane (37 mg). The mixture is stirred for 12 hour at 100° C. The mixture is diluted with water, acidified with 1 M aqueous HCl solution and extracted twice with ethyl acetate. The combined organic phases are washed with water and brine, dried (MgSO4) and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate/methanol 80:20:0→0:80:20) to give the title compound. Yield: 31 mg; LC (method 7): tR=1.16 min; Mass spectrum (ESI+): m/z=579 [M+H]+.

1. extractionextracted twice with ethyl acetate
2. washThe combined organic phases are washed with water and brine
3. dry with materialdried (MgSO4)
4. concentrationconcentrated
5. customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate/methanol 80:20:0→0:80:20)