反应详情

To a solution of 6-[{4-[(4-butylphenyl)ethynyl]benzyl}(hexyl)amino]-2,2-dimethyl-4H-1,3-benzodioxin-4-one (4.41 g, 8.4 mmol) in MeOH (500 mL) and water (30 mL) was added an aqueous solution of NaOH (7.0 mL, 5N). The reaction mixture was stirred at rt for 2 hrs and a yellow powder precipitated out progressively. Filtration and washing with water (2×) gave the title compound as a yellow powder. HPLC, Rt: 5.3 min (purity: 98.7%). LC/MS, M+(ESI): 498.3. 1H NMR (CDCl3) δ: 10.16 (s, 1H), 7.45 (m, 4H), 7.19 (m, 5H), 6.94 (dd, J=9.0, 3.0 Hz, 1H), 6.86 (d, J=9.0 Hz, 1H), 4.43 (s, 2H), 3.92 (s, 3H), 3.28 (t, J=7.5 Hz, 2H), 2.63 (t, J=7.5 Hz, 2H), 1.60 (m, 4H), 1.30 (m, 8H), 0.92 (m, 6H).

1. customa yellow powder precipitated out progressively
2. filtrationFiltration
3. washwashing with water (2×)