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594306435(金币+5, 翻译EPI+1): thanks 2011-03-10 19:35:19
将a与3mL Eaton 试剂混合, 在80 ℃油浴条件下加热反应3 h,冷却, 搅拌下倒入冰水中, 用冷的饱和碳酸氢钠水溶液中和至pH为6左右, 用乙醚提取五次, 合并提取液, 用饱和碳酸氢钠水溶液洗涤两次, 再用水洗两次, 分出有机层, 用无水硫酸钠干燥, 减压挥发溶剂, 残留固体用90%的乙醇重结晶得绿色针状晶体
a was mixed with 3 mL of Eaton and heated at 80 ℃ in an oil bath for 3hrs, cooled down, poured into the ice-water, make pH=6 with saturared NaHCO3 aq,
extracthed with ether for 5 times. the oganic layer was combined and washed with saturated NaHCO3 aq twice adn water twice,the organic was then dried with anhydrous sodium sulfate,evaporated and the residue was recrystallized with ethanol(90%) to get a green acicular crystal . |
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