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note
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3 (208 mg, 0.25 mmol) and NaOAc methanolic solution (1.0 M, 20 mL) were added to the residue, and the resulting solution was heated at 75 °C for 24 h. After cooling to rt, the solution was diluted with water (50 mL), and extracted with ethyl acetate (50 mL). The ethyl acetate phase was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The crude product was purified by chromatography on silica gel eluting with 10:90 methanol/ethyl acetate to give the expected product in 17-41% yields.
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26
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63149155739
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note
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6): 2.09-2.21 (m, 1H), 2.81-2.92 (m, 1H), 2.95-3.03 (m, 1H), 3.14-3.24 (m, 1H), 3.60-3.71 (m, 1H), 3.83 (s, 3H), 3.85-4.03 (m, 2H), 4.34-4.44 (m, 1H), 6.97 (d, J = 8.1 Hz, 1H), 7.07 (dd, J = 8.9, 2.3 Hz, 1H), 7.42 (d, J = 8.0 Hz, 1H), 7.57 (d, J = 1.5 Hz, 1H), 7.60 (d, J = 2.3 Hz, 1H), 7.84 (d, J = 8.9 Hz, 1H), 9.45 (s, 1H).
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27
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63149167457
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note
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2 (M+H) 576.0426, found 576.0432.
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28
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63149181019
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Kagotani, H. Japan Patent 2000219674, 2000.
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