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2-羟基-2-甲基-1-苯基丙酮的合成
Synthesis of 2-Hydroxy-2-methyl-1-propiophenone
【摘要】 以苯甲醛、镁、2 -溴丙烷、溴等为主要原料 ,经四步反应合成了光敏引发剂 2 -羟基 - 2 -甲基 - 1 -苯基丙酮。在 0°C时 ,将 1 6.5g苯甲醛滴加到由 4g Mg和 2 0 .6g2 -溴丙烷制得的 Grignard试剂中 ,在室温下搅拌 0 .5h,得到 2 0 .5g异丙基苯甲醇。将 2 5g K2 Cr2 O7、1 1 0 m L水和 2 0 m L浓H2 SO4 的混合液加入由 90 m L氯仿、5m L新洁而灭和 35g异丙基苯甲醇组成的混合液中 ,加完后 ,在室温下继续搅拌 2 h,得到 2 9.5g异丙基苯甲酮。在 65~ 75°C,将 32 .5g Br2 和 30 m L四氯化碳滴加到 60 m L CCl4 、1 5m L醋酸和 2 8.5g异丙基苯甲酮中 ,在温度不超过 70°C时搅拌 3h,得到α-溴代异丙基苯甲酮。1 0 gα-溴代异丙基苯甲酮、32 m L质量分数为 1 0 %的 Na OH溶液及 5m L新洁而灭 ,加热回流 3h,得到 6.8g 2 -羟基 - 2 -甲基 - 1 -苯基丙酮。
【Abstract】 Hydroxy 2 methyl 1 propiophenone was synthesized in four steps with benzaldehyde, 2 bromopropane and bromine as main raw materials. 16.5 g Benzaldehyde was added dropwise at 0 °C to a Grignard reagent from 4 g Mg and 20.6 g 2 Bromopropane, and the mixture stirred 0.5 h at room temperature, yield, 20.5 g isopropylphenylcarbinol (Ⅰ). A mixture of 25 g K 2Cr 2O 7, 110 mL H 2O and 20 mL concentrated H 2SO 4 was added slowly to 90 mL CHCl 3, 5 mL benzalkonium bromide solution and 35 g(Ⅰ) under 30 °C , the reaction mixture was stirred 2 h after added at room temperature, and produced 29.5 g isopropyl phenylketone (Ⅱ). 32 g Br 2 and 30 mL CCl 4 was dropped to the mixture from 60 mL CCl 4, 15 mL HOAc and 28.5 g (Ⅱ) at 65 °C ~75 °C , the reaction mixture was stirred 3 h at 70 °C , yielded 38.5 g α bromoisopropyl phenylketone (Ⅲ), 10 g (Ⅲ), 32 mL/10% (NaOH) and 5 mL benzalkonium bromide solution were refluxed 3 h, gave 6.8 g 2 hydroxy 2 methyl 1 propiophenone.
【Key words】 photosensitized initiator; 2 hydroxy 2 methyl 1 propiophenone; synthesis;
- 【文献出处】 化学世界 ,Huaxue Shijie (Chemical World) , 编辑部邮箱 ,2001年04期
- 【分类号】O625
- 【被引频次】7
- 【下载频次】443