反应详情

A procedure similar to step 3 of Example 1 was used. 1-(4-methoxy-phenyl)-4-phenyl-butan-1-one prepared in the step 2 and bromide were used as starting materials, and anhydrous AlCl3 was used as catalyst. The crude product obtained was recrystallized with a mixture of petroleum ether and ethyl acetate (2:1) to give a product as a white solid in a yield of 89.4%, mp: 65-66 └. 1H-NMR (CDCl3, 400 MHz) δ: 2.38˜2.52 (2H, m, CH2), 2.75˜2.90 (2H, m, CH2), 3.88 (3H, s, OCH3), 5.03 (1H, t, J=8.00 Hz, CHBr), 6.93 (2H, d, J=9.2 Hz, ArH), 7.18˜7.32 (5H, m, ArH), 7.91 (2H, d, J=9.20 Hz, ArH); ESI-MS m/e (%): 334.0 (M+2, 1), 332.0 (M, 1), 229.9 (53), 227.9 (53), 135.0 (100).

1. customThe crude product obtained
2. customwas recrystallized with a mixture of petroleum ether and ethyl acetate (2:1)