反应详情

In two batches, 81.4 mg (0.016 mmol) of the compound from Example 335B above was dissolved in 2 mL of methanol to which 14.9 μL of trimethylsilyl chloride was added and stirred for 2 hours. The solvent was removed and the crude product chromatographed on silica gel, eluting with 2% and 5% methanol in methylene chloride. The solvent was removed and the product dried to afford 42.6 mg of the title compound. MS M/Z (DCI/NH3): 461 (M+H), 478 (M+NH4). Proton NMR (DMSO):δ 1.46 (t, 2H), 2.53-2.77 (4H), 3.45 (m, 3H), 3.55 (d, 1H), 3.64-3.92 (6H), 4.64 (m, 2H), 6.65 (d, 1H), 6.94 (d, 1H), 7.07-7.27 (10H). Anal calc. for C24H32N2O7.H2O: C, 60.25; H, 7.11; N, 5.86; found: C, 60.38; H, 6.56; N, 5.86.

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