反应详情

A procedure similar to step 5 of Example 6 was used. 2-bromo-3-(4-fluoro-phenyl)-1-(4-methoxy-phenyl)-propan-1-one prepared in the step 3, thiourea and anhydrous sodium acetate were used as starting materials, refluxed for 2 hours, hold overnight, filtered, washed with water, and dried to obtain a product. A single spot was shown by TLC. The product was not further purified. The product was a white solid in a yield of 81.9%, mp: 199-201 └. 1H-NMR (DMSO-d6, 400 MHz) δ: 3.76 (3H, s, OCH3), 4.03 (2H, s, CH2), 6.84 (2H, s, NH2), 6.94 (2H, d, J=8.96 Hz, ArH), 7.13 (2H, t, 3JFH=3JHH=8.96 Hz, ArH), 7.23 (2H, dd, 3JHH=8.72, 4JFH=5.64 Hz, ArH), 7.46 (2H, d, J=8.96 Hz, ArH); EI-MS m/e (%): 314.2 (M+, 100), 109.1 (12); HREI-MS Calcd. for C17H15FN2OS: 314.0889. found: 314.0890. Anal. Calcd. for C17H15FN2OS: C, 64.95; H, 4.81; N, 8.91. found: C, 65.10; H, 5.24; N, 8.98.

1. temperaturerefluxed for 2 hours
2. filtrationfiltered
3. washwashed with water
4. customdried
5. customto obtain a product