反应详情

A stirred solution of 4-(3-cyclopentyloxy-4-methoxyphenyl)-1,1-(ethylenedioxy)-4-(2-[4-(1-piperidinocarbonylmethoxy)phenyl]ethynyl)cyclohexane (0.232 g, 0.40 mmol) in tetrahydrofuran (9 mL) was treated with 3N hydrochloric acid (0.90 mL) as described in Example 12 above. The crude product was purified by chromatography (silica, 50% ethyl acetate/hexanes) and the solvent removed in vacuo to afford the titled compound as a resin (0.127 g, 59%). Anal. (C28H30O5.1/10 H2O) calcd: C 75.01, H 6.79, found: C 74.97, H 6.87. 1H-NMR (400 MHz, CDCl3) δ 7.41 (d, J=9.1 Hz, 2H), 7.22 (d, J=2.3 Hz, 1H), 7.11 (d-d, J=8.4 Hz, J=2.3 Hz, 1H), 6.92 (d, J=8.6, 1H), 6.86 (d, J=8.5, 1H),4.80 (p, 1H), 4.70 (s, 2H), 4.00 (s, 4H), 3.85 (s, 3H), 3.56 (t, J=5.5 Hz, 2H), 3.48 (t, J=5.5 Hz, 2H), 3.03 (d-t, J=6.1 Hz, J=14.3, 2H), 2.47 (d,br, J=14.9, 2H), 2.4-2.2 (m, 4H), 2.0 to 1.5 (m, 25H with H2O).

1. customThe crude product was purified by chromatography (silica, 50% ethyl acetate/hexanes)
2. customthe solvent removed in vacuo