反应详情

A procedure similar to step 5 of Example 6 was used. 2-bromo-1-(4-methoxy-phenyl)-hexan-1-one prepared in the step 3, thiourea and anhydrous sodium acetate were used as starting materials, refluxed for 3 hours, followed by post-treatment to give a crude product, which was recrystallized with petroleum ether and ethyl acetate at a ratio of 1:1 (V:V) to obtain a product as a white solid in a yield of 57.2%, mp: 118-119 └. 1H-NMR (CDCl3, 400 M.Hz) δ: 0.90 (3H, t, J=7.2 Hz, CH3), 1.36 (2H, sextuple, J=7.20 Hz, CH2), 1.59 (2H, quintuple, J=7.20 Hz, CH2), 2.74 (2H, t, J=7.2 Hz, CH3), 3.83 (3H, s, OCH3), 4.93 (2H, br, NH2), 6.93 (2H, d, J=8.80 Hz, ArH), 7.45 (2H, d, J=8.80 Hz, ArH); EI-MS m/e (%): 262.0 (M+, 55), 219.0 (100), 177.0 (36); HREI-MS Calcd. for C14H18N2OS: 262.1140. found: 262.1140. Anal. Calcd. for C14H18N2OS: C, 64.09; H, 6.92; N, 10.68. found: C, 64.19; H, 7.02; N, 10.63.

1. temperaturerefluxed for 3 hours
2. customto give a crude product, which
3. customwas recrystallized with petroleum ether and ethyl acetate at a ratio of 1:1 (V:V)