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shuoli金虫 (小有名气)
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Sodium hydroxide was dissolved in an appropriate amount of distilled water. This solution was heated in a water bath at 80–90◦C; agar agar was then slowly added to the hot alkali solution with stirring till a brown transparent viscous solution was obtained. This solution on cooling in ice gave a gel. The quantities of the three components, namely water–NaOH–agar agar, were varied to get different types of gels. Results are plotted on the triangular phase diagram. For the required GEBC a gel with the following composition was prepared: in 6 g of water 1 g of NaOH was dissolved with stirring. This solution was heated in a water bath at a temperature of about 80–90◦C; to this hot solution, 3 g of agar agar powder was slowly added while stirring the mixture homogeneously. The heating and stirring were continued till a translucent brown viscous solution was obtained, which on cooling in ice gave a hard solid gel which could be cut into pieces. To acrylonitrile (10 mmol), in the alcohol (20 ml) taken in excess, 10% NaOH-GEBC pieces (0.1 g) were added. The reaction mixture was stirred at the required temperature. For 1aand 1bthe reactions were moni-tored over GC by drawing samples from the reaction and analyzing them. In case of other alcohols, however, the reaction took at least 3 h. The solution was then filtered, the GEBC was washed with the alcohol used and the filtrate was analyzed by G.C. In the case of benzyl alcohol, the alcohol and acrylonitrile were taken in 1:1 mole ratio in 2-methylpropan-2-ol as solvent (5 ml) and the reaction was carried out at 50◦C. The identity of known cyanoethylated products of methanol, ethanol, cellosolve, and benzyl alcohol was established by their b.p.s and FT-IR spectra. The identity of unreported cyanoethylated products of 1-propanol and 2-methylpropan-1-ol was established with the help of 1H NMR spectra. |
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爱与雨下: 金币+2 2013-05-28 21:53:22
shuoli: 金币+50, 翻译EPI+1, ★★★很有帮助 2013-05-28 22:25:05
爱与雨下: 金币+2 2013-05-28 21:53:22
shuoli: 金币+50, 翻译EPI+1, ★★★很有帮助 2013-05-28 22:25:05
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用适量的蒸馏水溶解氢氧化钠。将上述溶液置于80-90℃水浴中加热；然后将琼脂慢慢添加到热碱溶液中并搅拌直到变为棕色透明粘稠溶液。该溶液在冰中冷却后得到凝胶。这三个成分（即水、氢氧化钠、琼脂）的数量不同导致所得凝胶的类型不同。结果绘制在三角相图中。 所需的凝胶包埋碱催化剂凝胶由以下成分制备: 1g氢氧化钠在6g水中搅拌溶解。将该溶液置于80-90℃水浴中加热；将3g琼脂粉缓慢加入到该热溶液中，搅拌直到混合均匀。溶液持续加热并搅拌直到变为半透明的棕色粘稠溶液，在冰中冷却后得到可切成片的硬固体凝胶。 丙烯腈(10mmol)加入到过量的乙醇(20ml)中,再加入10%的NaOH-凝胶包埋碱催化剂片(0.1g)。反应物在所需温度下搅拌。1a和1b反应利用气相层析来检测，从反应中取样并分析它们。然而，对于其他醇类，反应至少要进行3h。溶液过滤，用乙醇洗涤凝胶包埋碱催化剂并用气相层析分析了滤液。 苯甲醇、乙醇和丙烯腈按照摩尔比1:1分别置于溶剂2-甲基丙烷-2-醇(5ml)中在50℃下进行反应。 已知标识的甲醇,乙醇,甲基纤维素和苄醇的氰乙基化产品通过其叔丁基二苯基硅烷基和傅里叶变换红外光谱加以证明。未知标识的2-甲基丙烷-1-醇和1-丙醇的氰乙基化产品通过核磁氢谱的辅助加以证明。 |
2楼2013-05-28 20:04:59
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