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tosn铁杆木虫 (职业作家)
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求大侠翻译，见 EXAMPLE 1 This example describes the preparation of diethyl pyrocarbonate with PEG 15 stearamine as the catalyst. A solution of ethyl chloroform ate (114.2 grams(95%) 1.00 mole) and PEG-15 stearamine (1.88 grams (99%) 0.002 mole) was introduce to a 1000 milliliter,three-necked reaction flask with a bottom stopcock. The reaction flask was equipped with a mechanical teflon blade stirrer, sodium hydroxide solution inlet, vent and thermowell for a thermocouple, which was connected to a temperature control unit. Sodium hydroxide was charged to the reaction flask through a Masterflex addition pump. The temperature control unit activated a cooling water pump which directed ice water against the reaction flask and also controlled the Masterflex pump so as to maintain the reaction temperature at below 15° C. When the temperature in the reaction flask was below 15° C., sodium hydroxide solution was charged to the flask. When the temperature rose above 15° C., the Masterflex pump was shut off and ice water sprayed on the reaction flask to cool the contents of the reaction flask. Aqueous sodium hydroxide solution (82 grams (50%) 1.025 moles) was charged to the reaction flask over a period of approximately 60 minutes. Semi-solids which remained on the sides of the flask were rinsed into the liquid reaction mixture with a small amount of water and the reaction mixture post stirred at 15° C. for minutes. 125.5 grams of water (including the amount of rinse water) was added tot he reaction flask so that the theoretical percent solids in the aqueous phase was about 25 percent. The reaction mixture was agitated from 10seconds to dissolve all solids before phase separation was performed. The top organic phase (82.7 grams) was dried over 6.2 grams of magnesium sulfate to give a light yellow clear liquid (77.2 grams). Volatiles in the yellow liquid product were removed by a rotary evaporator under water aspirator vacuum (40 mm/Hg) for 60 minutes at 60° c., and then under vacuum pump (< 2 mrn/Hg) for 60 minutes at 60° C., thereby to obtain a final liquid product (71.8 grams). This product was a clear, light yellow liquid having an APHA color of 100.The conversion of chloroformate to chloride anion (CI-) was found to be 100percent based on the analysis for (CI-) in the aqueous phase. The infrared spectrum of the product matched the literature infrared spectrum for diethyl pyrocarbonate with a characteristic band at 1823em-1. Both 1H (proton) and BC nuclear magnetic resonance analysis supported the product as being diethyl pyrocarbonate with a minor amount of diethyl carbonate. The product has an assay of 96 percent as determined by gas chromatograph analysis 拜托拜托！！！ |
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南京工大
木虫 (小有名气)
- 翻译EPI: 14
- 应助: 0 (幼儿园)
- 金币: 1971.3
- 散金: 102
- 红花: 6
- 帖子: 173
- 在线: 81.1小时
- 虫号: 1410020
- 注册: 2011-09-20
- 性别: GG
- 专业: 高分子组装与超分子结构
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tosn: 金币+50, 翻译EPI+1, ★★★★★最佳答案, xiexi 2013-04-24 22:00:48
tosn: 金币+50, 翻译EPI+1, ★★★★★最佳答案, xiexi 2013-04-24 22:00:48
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这一实例描述了使用硬脂胺聚氧乙烯醚作为催化剂制备焦碳酸二乙酯的过程。氯甲酸乙酯（114.2 g，95%，1 mol）溶液和硬脂胺聚氧乙烯醚（1.88 g，99%，0.002 mol）加入到底部带有活塞的1000毫升的三口烧瓶中。烧瓶配有一个特氟龙材质的桨式搅拌器，一个氢氧化钠溶液的加入口和出口，以及一个套管用于安装热电偶，热电偶接在控温装置上。氢氧化钠溶液通过Masterflex蠕动泵滴加入反应体系。控温装置与一个冷却水泵相连，可以控制冰水的流出以冷却反应装置，还可以控制蠕动泵的流速以使得反应温度在15°C以下。 当反应装置中的温度在15°C以下时，氢氧化钠溶液就被加入到烧瓶中。当温度升高到15°C以上时，蠕动泵停止工作，冰水被喷射到反应装置上以降低反应物温度。 氢氧化钠溶液（82 g，50%，1.025 mol）应在60分钟左右的时间内被加入到反应装置中。反应结束后，粘在烧瓶壁上的少量半固体物质可以用少量的水冲洗到液相反应混合物中，并保持在15°C下继续搅拌几分钟。向装置中加入125.5 g水（含冲洗所用的水），这样液相中理论的固含量即为25%。在相分离现象发生前，摇晃反应混合物约10秒钟以使得所有固体溶解。 使用6.2g无水硫酸镁对上层的有机相（82.7 g）进行脱水，得到了浅黄色的清澈液体（77.2 g）。该液体中的易挥发组分通过使用旋转蒸发仪，先在水泵抽真空条件（40 mm/Hg）下60°C旋转蒸发60分钟，接着再在真空泵作用下（<2 mm/Hg）60°C旋转蒸发60分钟除去，最终得到液相的产物（71.8 g）。该产物为淡黄色的清澈液体，色度为100。通过对液相产物的分析可知，氯甲酸酯中的氯元素的转化率为100%。产物的红外光谱与文献中焦碳酸二乙酯的光谱一致，在1823 em-1处有特征峰。1H和BC的核磁共振分析都证实了该产物为焦碳酸二乙酯，其中含有很少量的碳酸二乙酯。通过气相色谱分析，该产物的含量为96%。 |
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2楼2013-04-23 21:48:36