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[求助]
求翻译一段实验操作记录
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0.1 mole of 原料 was added dropwise to 0.25 mole of 二乙胺 (30% solution in abs. 乙醇) over a period of one hour. The reaction flask was immersed in ice water during the reaction and stirring was continued for one-half hour after the addition of the 原料.Then cold, conc. 盐酸 was added very slowly along with some finely cracked ice until the mixture was acidic. If it became warm the product turned very dark in color and a larger proportion of tar war produced. At this point the reaction mixture was orange or red dur to the presence of some原料that hasn't reacted and to formation of certain tarry by-products. These were extracted with ether from the water layer and the 原料 recovered. The water layer was evaporated to dryness in vacuo, treated with a little 氯仿and evaporated to dryness again to assist in removing the moiture from the rather hard mass. After standing in the vaccuum executor for one day, the residue was extracted several times with fresh portions of 氯仿 and each time the insoluble cysts of 二乙胺盐酸盐 were filtered. The 氯仿 solution was then evaporated until it was very concentrated,and acetone was added to cause the crystallisation of the 产物. Recrystallisation was carried out by dissolving in a small amount of 乙醇, filtering, and adding about twice the vol. of 丙酮 in small protions 。 |
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cfk580713
至尊木虫 (著名写手)
- 翻译EPI: 277
- 应助: 30 (小学生)
- 贵宾: 0.038
- 金币: 13604.3
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sltmac: 金币+30, 翻译EPI+1 2012-04-18 11:20:45
sltmac: 金币+30, 翻译EPI+1 2012-04-18 11:20:45
| 在1小时内将 0.1 摩尔 原料滴加到0.25 摩尔二乙胺中(无水乙醇中30 %的溶液) 。在反应过程中，反应瓶浸没于冰水中，并在原料滴加完后继续搅拌0.5 小时。之后，用冷却过的浓盐酸及碎冰缓慢调节反应体系至酸性。如果 体系升温会导致产品的颜色变黑，并且产生更多量的 tar war。此时，反应体系为桔色或红色，这是因为部分原料并没有反应完全并产生了部分焦油状的副产物。这些未反应的原料可以通过乙醚从水层中萃取出来进而回收利用。水层通过真空挥发(就是旋转蒸发)除去溶剂水，再用小量的氯仿处理，并再次旋干以确保除尽了其中的湿气。在真空烘箱中干燥一天后，所得到的固体用新蒸氯仿萃取数次，每次萃取时过滤除去不溶的二乙胺盐酸盐晶体。对所得到的 氯仿溶液进行浓缩，并加入丙酮以促使产物结晶析出。粗产品可以通过重结晶的方法进行提纯：将样品溶于少量乙醇，过滤后，分批加入两倍体积的丙酮。 |
2楼2012-04-16 23:08:43
