反应详情

To a 250 ml flask were added 10.8 g o-methylphenol, 26.0 g sodium thiocyanate, 70 ml methanol, added dropwise 100 ml methanol solution containing 10.3 g NaBr, 5.3 ml liquid bromine at 0° C. under N2 atmosphere. The mixture was stirred at room temperature for 3 hours. The mixture was neutralized with saturated NaHCO3 solution, extracted with CH2Cl2 for four times. The extract was dried over anhydrous Na2SO4, filtrated, evaporated and purified by column chromatograph (petroleum ether:ethyl acetate=8:1) to obtain 11.1 g yellow solid, yield 67.27%. 1H-NMR (400 MHz, CDCl3, δ ppm) δ 2.2558 (3H, s), 5.0 (1H, s), 6.8 (1H, d, J=8.4 Hz), 7.3605-7.2631 (1H, m), 7.3542 (1H, s).

1. extractionextracted with CH2Cl2 for four times
2. dry with materialThe extract was dried over anhydrous Na2SO4
3. filtrationfiltrated
4. customevaporated
5. custompurified by column chromatograph (petroleum ether:ethyl acetate=8:1)