反应详情

To a solution of 3 (10.00 g, 39 mmol) in 4:1 ether/i-PrOH (100 mL) was added dropwise conc. aqueous HCl (3.5 mL, 1.1 equiv.). Upon stirring for 10 minutes the suspension was diluted with ether (100 mL), filtered and the filter-cake was washed with ether (3×50 mL) and air-dried, affording 26 (11.40 g, 100%). 1H NMR (300 MHz, d6-DMSO) δ ppm 10.86 (s, 2H, NH), 7.52 (d, J=8.1 Hz, 2H, Ar), 7.23 (t, J=8.1 Hz, 1H, Ar), 5.20 (q, J=6.6 Hz, 1H) 3.87 (s, br, 4H), 1.66 (d, J=6.6 Hz, 3H); 13C NMR (75 MHz, d6-DMSO) δ ppm 169.5, 149.2, 130.3, 129.1, 127.5, 73.9, 45.2, 19.5; mp=226-227° C.; [α]23D=−39.0° (c 1.0, EtOH) (lit.5 [α]20D −34.5° (c 1.0, EtOH).

1. filtrationfiltered
2. washthe filter-cake was washed with ether (3×50 mL)
3. customair-dried