反应详情

温度

80 °C

To a stirred solution of the product from Step A (0.24 g, 0.59 mmol) was added 2-(methyamino)ethanol (2.0 mL) and the solution was heated at 80° C. for 18 h. A saturated aqueous solution of ammonium chloride (20 mL) was added to the reaction mixture, which was extracted with ethyl acetate (3×50 mL). The combined extracts were washed with brine (10 mL), dried (MgSO4) and evaporated to give a residue which was purified by chromatography (silica, 30% ethyl acetate in hexane) to give an oil (0.16 g, 68%): 1H NMR (CDCl3) δ 8.50 (1H, brs), 8.01 (1H, s), 7.30 (6H, m), 6.77 (1H, d, J=8.4 Hz), 5.02 (2H, m), 4.59 (2H, m), 4.77 (1H, brs), 4.09 (1H, m), 3.69 (1H, m), 3.36 (2H, m), 2.93 (3H, s), 1.26 (3H, d, J=6.4 Hz); MS (ES) m/z 399 (M+).

1. extractionwas extracted with ethyl acetate (3×50 mL)
2. washThe combined extracts were washed with brine (10 mL)
3. dry with materialdried (MgSO4)
4. customevaporated
5. customto give a residue which
6. customwas purified by chromatography (silica, 30% ethyl acetate in hexane)