3.
乙酰乙酸乙酯是有机合成的中间体,用乙酸乙酯合成乙酰乙酸乙酯的原理如下:
![](https://math.21cnjy.com/MathMLToImage?mml=%3Cmath+xmlns%3D%22http%3A%2F%2Fwww.w3.org%2F1998%2FMath%2FMathML%22%3E%3Cmtext%3EC%3C%2Fmtext%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EH%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E3%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmtext%3EC%3C%2Fmtext%3E%3Cmtext%3EO%3C%2Fmtext%3E%3Cmtext%3EO%3C%2Fmtext%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EC%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E2%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EH%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E5%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmo%3E%2B%3C%2Fmo%3E%3Cmtext%3EC%3C%2Fmtext%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EH%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E3%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmtext%3EC%3C%2Fmtext%3E%3Cmtext%3EO%3C%2Fmtext%3E%3Cmtext%3EO%3C%2Fmtext%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EC%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E2%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EH%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E5%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmunderover%3E%3Cmo%3E%E2%87%8C%3C%2Fmo%3E%3Cmrow%3E%3Cmtext%3EC%3C%2Fmtext%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EH%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E3%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmtext%3EC%3C%2Fmtext%3E%3Cmtext%3EO%3C%2Fmtext%3E%3Cmtext%3EO%3C%2Fmtext%3E%3Cmtext%3EH%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EC%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E2%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EH%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E5%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmtext%3EO%3C%2Fmtext%3E%3Cmtext%3EN%3C%2Fmtext%3E%3Cmtext%3Ea%3C%2Fmtext%3E%3C%2Fmrow%3E%3C%2Fmunderover%3E%3Cmtext%3EC%3C%2Fmtext%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EH%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E3%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmover%3E%3Cmrow%3E%3Cmtext%3EC%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmunder%3E%3Cmrow%3E%3Cmtext%3EO%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmtext%3E%7C%3C%2Fmtext%3E%3Cmtext%3E%7C%3C%2Fmtext%3E%3C%2Fmrow%3E%3C%2Fmunder%3E%3C%2Fmrow%3E%3C%2Fmover%3E%3Cmo%3E%E2%88%92%3C%2Fmo%3E%3Cmtext%3EC%3C%2Fmtext%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EH%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E2%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmtext%3EC%3C%2Fmtext%3E%3Cmtext%3EO%3C%2Fmtext%3E%3Cmtext%3EO%3C%2Fmtext%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EC%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E2%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EH%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E5%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmo%3E%2B%3C%2Fmo%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EC%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E2%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EH%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E5%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmtext%3EO%3C%2Fmtext%3E%3Cmtext%3EH%3C%2Fmtext%3E%3C%2Fmath%3E)
主要反应试剂及产物的物理常数如下表:
名称 | 熔点 | 沸点 | 密度 | 溶解度 |
![](https://math.21cnjy.com/MathMLToImage?mml=%3Cmath+xmlns%3D%22http%3A%2F%2Fwww.w3.org%2F1998%2FMath%2FMathML%22%3E%3Cmsub%3E%3Cmrow%3E%3Cmtext%3EH%3C%2Fmtext%3E%3C%2Fmrow%3E%3Cmrow%3E%3Cmn%3E2%3C%2Fmn%3E%3C%2Fmrow%3E%3C%2Fmsub%3E%3Cmtext%3EO%3C%2Fmtext%3E%3C%2Fmath%3E)
| 乙醇 | 乙醚 |
苯 | 5.5 | 80.1 | 0.88 | 不溶 | 互溶 | 互溶 |
二甲苯 | ![](https://math.21cnjy.com/MathMLToImage?mml=%3Cmath+xmlns%3D%22http%3A%2F%2Fwww.w3.org%2F1998%2FMath%2FMathML%22%3E%3Cmo%3E%E2%88%92%3C%2Fmo%3E%3Cmn%3E2%3C%2Fmn%3E%3Cmn%3E5%3C%2Fmn%3E%3Cmn%3E.%3C%2Fmn%3E%3Cmn%3E1%3C%2Fmn%3E%3Cmn%3E8%3C%2Fmn%3E%3C%2Fmath%3E)
| 144.4 | 0.8802 | 不溶 | 互溶 | 互溶 |
乙酸乙酯 | ![](https://math.21cnjy.com/MathMLToImage?mml=%3Cmath+xmlns%3D%22http%3A%2F%2Fwww.w3.org%2F1998%2FMath%2FMathML%22%3E%3Cmo%3E%E2%88%92%3C%2Fmo%3E%3Cmn%3E8%3C%2Fmn%3E%3Cmn%3E3%3C%2Fmn%3E%3Cmn%3E.%3C%2Fmn%3E%3Cmn%3E6%3C%2Fmn%3E%3C%2Fmath%3E)
| 77.1 | 0.9003 | 难溶 | 互溶 | 互溶 |
金属钠 | 97.82 | 881.4 | 0.968 | 反应 | 反应 | 不溶 |
乙酰乙酸乙酯 | ![](https://math.21cnjy.com/MathMLToImage?mml=%3Cmath+xmlns%3D%22http%3A%2F%2Fwww.w3.org%2F1998%2FMath%2FMathML%22%3E%3Cmo%3E%26lt%3B%3C%2Fmo%3E%3Cmo%3E%E2%88%92%3C%2Fmo%3E%3Cmn%3E8%3C%2Fmn%3E%3Cmn%3E0%3C%2Fmn%3E%3C%2Fmath%3E)
| 180.4 | 1.0282 | 微溶 | 互溶 | 互溶 |
已知:乙酰乙酸乙酯在95℃开始分解。
现用乙酸乙酯(含
乙醇)合成乙酰乙酸乙酯的步骤如下:
①制钠珠:将
金属
迅速切成薄片,放入
的三颈烧瓶中,并加入
经过干燥的溶剂A,加热回流至熔融,装置如图1,拆去回流装置,用橡皮塞塞住瓶口,用力振摇即得细粒状钠珠。稍冷分离回收溶剂A。
![](http://tikupic.21cnjy.com/2024/04/14/2a/a3/2aa3252b82e0565504ebc5bf5acbd192_320x274.png)
②加酯回流:从图2装置的恒压滴液漏斗中加入10mL乙酸乙酯于盛有钠珠的三颈烧瓶中,装上回流装置,开启电磁搅拌棒,回流至钠消失,得橘红色溶液。
③酸化:向橘红色溶液中加入50%醋酸使其呈弱酸性(
)。
④分液:将反应液转入分液漏斗,加入等体积的饱和氯化钠溶液,振摇,静置,分液。将有机层倒入锥形瓶中,并加适量的无水
充分振荡。
⑤蒸馏:将步骤④所得有机混合液水浴加热蒸馏出未反应的乙酸乙酯,停止蒸馏,冷却。再将蒸馏得到的剩余物进行减压蒸馏,收集馏分。
回答下列问题: