问题：帮忙修改并完善一下翻译
类型：求助 (悬赏分:3分)
提问：quick208
等级：▲
版块：有机化学问题(jimuwei,fpcwin1211,netpanda,yjgzfl,Ftian,)
信誉：95%
回复：8
阅读：1239
时间：2008-07-06 18:04:28 编辑加入/取消收藏订制/取消短消息举报该贴

Into a 250 cm3, twonecked
flask, equipped with a reflux condenser and a dropping
funnel were charged cyclohexanone (4.91 g, 5.2 cm3, 50 mmol),
phenethylamine (5.45 g, 5.65 cm3, 45 mmol), Et,N (15.18 g,
20.9 cm3, 150 mmol) and MeOH (60 cm3). The mixture was
stirred magnetically and cooled (water bath), while AcOH (12.0
g, 11.45 cm3, 200 mmol) was added with a pipette below the
surface of the liquid. The dropping funnel was also charged
with AcOH (12.0 g, 11.45 cm3, 200 mmol) in MeOH (10 cm3).
Finally, Mg (5.47 g, 225 mmol) was added to the mixture which
was then stirred vigorously (I 200-1 800 rpm, large stirring bar),
under reflux, for 2 h. After this, AcOH was added, portionwise,
from the dropping funnel, over a 2 h period. After a further
period under reflux ( I h), the mixture was cooled to 20-25 "C
and filtered with a medium porosity sinter funnel. The
precipitate was removed from the funnel and stirred
magnetically with MeOH (50 cm3) for 5 min before it was again
filtered. Finally, it was washed, with thorough manual stirring
on the funnel, with Et,O (70 cm3). If the combined filtrate
contained some precipitate, it was filtered through a less porous
sinter funnel. A solution of K,CO, (15 g) and EDTA disodium
salt (3.0 g) in water (70 cm3) was added to the filtrate, and the
mixture concentrated on a rotatory evaporator (20-25 "C, 25
min). The resulting emulsion was extracted with Et,O (3 x 70
cm3) and the combined extracts were dried (K,CO,) and
evaporated. The residue was dissolved in MeOH (20 cm3) and
added slowly, with magnetic stirring, to the solution of anh.
oxalic acid (5.40 g, 60 mmol) in MeOH (50 cm3). The mixture
was cooled to - 20 "C after which the precipitated monooxalatesalt was filtered off, washed with Et,O (50 cm3), and dried
(80 "C, 6 h). It may be recrystallized from hot methanol; yield
10.45 g (79%, calculated with reference to the 2-phenylethyamine
used). The free amine was obtained by treatment
of the oxalate salt with K,C03 (20 g) in water (100 cm3) and
extraction with CH2C12 (2 x 50 cm3). The combined extracts
were dried (K,CO,), and evaporated (rotatory evaporator) and
the residue was vacuum distilled, to afford the pure amine (6.92
g, 7573, bp 148-155 "C/12 Torr.

3A加入到250mL的两颈瓶中，两颈瓶上分别装有回流冷凝管和滴液漏斗。通过滴液漏斗将环已酮，苯乙胺，Et2O，甲醇加入其中。混合液在磁力搅拌下，水浴中冷却下，将乙醇通过插入液面下的管子加入其中。最后加入Mg，回流条件下，快速搅拌2h。之后再加入甲醇，通过分液漏斗，滴加超过2h,再回流1h,冷却到20-25度，过滤，固体用甲醇溶解，搅拌5分钟后再过滤，k2CO3,EDTA溶于水，加入到滤液中，在20-25度浓缩，固体用乙酸乙酯萃取，KCO3干燥浓缩，固体溶于甲醇，再慢慢加入到搅拌的甲醇和季胺酸盐溶液中，冷却至-20度，过滤掉单氧化的盐，乙酸乙酯淋洗，干燥，甲醇重结晶

这样翻译对么？请大家修改和完善一下

回复人：quick208,▲ (以父之名) 时间：2008-07-07 10:41:37 编辑	1楼
我就是觉得有点乱所以叫大家帮忙

回复人：hichemcz40,▲▲ (认真做人、踏实做事！) 时间：2008-07-06 18:12:46 编辑	2楼
有点乱。自己整理一下可以了。

回复人：afc,★★ (氟化学产品) 时间：2008-07-07 12:11:31 编辑

3楼

由于文献分子式不清楚，要结合原文看！

在配有冷凝器和滴加漏斗的250毫升的两口烧瓶内，加入环已酮(4.91 g, 5.2 cm3, 50 mmol)，苯乙胺(5.45 g, 5.65 cm3, 45 mmol)，Et,N (15.18 g,20.9 cm3, 150 mmol)，甲醇(60 cm3)。开动搅拌，水浴冷却，将乙酸（12.0g, 11.45 cm3, 200 mmol)用移液管加入到液面下。滴加漏斗内装入溶于甲醇(10 cm3)中的乙酸(12.0 g, 11.45 cm3, 200 mmol)溶液。最后，将Mg (5.47 g, 225 mmol)加入到混合物内，强烈搅拌(1200-1 800 转/分, 大搅拌棒)，回流反应2小时。之后，将乙酸用2小时的时间分批加入，加毕，继续回流1小时。然后，冷却到20-25度，用一个中等孔隙的漏斗过滤。将滤饼取出，加入甲醇(50 cm3)，搅拌5分钟，再次过滤，最后，再漏斗内，边人工搅拌，边用Et,O (70 cm3)洗滤饼。如果合并的滤液含有沉淀，再用小一点孔径的漏斗过滤。将K,CO, (15 g)和EDTA钠盐(3.0 g)溶于水(70 cm3)的溶液加入到滤液内，将混合物在旋转蒸发器上浓缩(20-25 "C, 25min)，浓缩液用Et,O (3 x 70cm3)萃取三次，合并的萃取液用(K,CO,)干燥，浓缩。剩余物溶于甲醇(20 cm3)内，在搅拌下，将其慢慢加入到溶于甲醇(50 cm3)中的草酸(5.40 g, 60 mmol)的溶液中，冷却至20度，过滤得单草酸盐，用Et,O (50 cm3)洗，干燥(80 "C, 6 h)。也可以用热甲醇重结晶，得到10.45 g（以苯乙胺计，收率79%）。用碳酸钾的水溶液处理草酸盐，用二氯甲烷萃取(2 x 50 cm3)，合并的萃取液干燥，浓缩，减压蒸馏，可得纯游离胺(6.92g, 7573, bp 148-155 "C/12 Torr).

回复人：quick208,▲ (以父之名) 时间：2008-07-07 12:44:17 编辑	4楼
已经打分了！

回复人：klair,▲ (向各位有学识有经验的老师学习！) 时间：2008-07-07 12:51:38 编辑	5楼
Et,N 应该是Et3N 吗

回复人：quick208,▲ (以父之名) 时间：2008-07-07 17:07:23 编辑	6楼
就第一个是Et3N 其余是Et20

回复人：quick208,▲ (以父之名) 时间：2008-07-07 17:05:34 编辑	7楼
对

回复人：quick208,▲ (以父之名) 时间：2008-08-06 10:51:34 编辑	8楼
222222222

得分人：afc :3,

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