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baishitou3

金虫 (小有名气)

[交流] 重金求化学合成翻译,高手进来指导指导

To a flame-dried
Schlenk test tube with a magnetic stirring bar was charged CuI
(38.2  mg,  0.2  mmol),  Cs 2 CO 3 (0.65  g,  2.0  mmol),  nitrogen-
containing heterocycle (1.4 mmol), aryl or heteroaryl halide (1.0
mmol), and DMF (2 mL) under N 2 . A rubber septum was replaced
with a glass stopper, and the system was then evacuated twice and
back filled with N 2 . The reaction mixture was stirred for 30 min at
room temperature, and then heated at 120 °C for 40 h. The reaction
mixture was then cooled to ambient temperature, diluted with 2-3
mL of ethyl acetate, filtered through a plug of silica gel, and washed
with 10-20 mL of ethyl acetate. The combined organic extracts
were concentrated, and the resulting residue was purified by column
chromatography on silica gel to provide the desired product.
以上是一段合成的步骤,filtered through a plug of silica gel, and washed
with 10-20 mL of ethyl acetate. The combined organic extracts
were concentrated,这一段非常的难懂啊,高手们进来看看,指导指导啊
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slowstar

木虫 (职业作家)

★ ★ ★ ★ ★ ★ ★ ★
发芽土豆(金币+2):谢谢参与 2010-09-23 09:46:24
baishitou3(金币+5): 2010-09-27 08:40:33
baishitou3(金币+2): 2010-10-04 22:06:17
ringzhu(金币+6): 2010-11-22 12:32:07
filtered through a plug of silica gel, and washed
with 10-20 mL of ethyl acetate.
The combined organic extracts were concentrated, and the resulting residue was purified by column
chromatography on silica gel to provide the desired product.
(在砂心漏斗或布氏漏斗里)先填上些硅胶,然后抽滤,再用10-20 mL乙酸乙酯淋洗。合并所得滤液(即抽滤和乙酸乙酯淋洗所得的滤液),将滤液浓缩(用旋转蒸发仪最方便了)后所得的剩余物过硅胶柱(即有机合成上俗称的过柱子),即可得到所需产物。
精韧不怠,日进有功
3楼2010-09-20 22:21:45
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cfk580713

至尊木虫 (著名写手)

★ ★ ★ ★
wypward(金币+1):谢谢参与 2010-09-20 20:49:10
baishitou3(金币+2, 翻译EPI+1): 2010-09-27 08:40:11
baishitou3(金币+2): 2010-10-04 22:06:22
ringzhu(金币+3): 2010-11-22 12:32:12
过滤除去不溶物吧,再用乙酸乙酯洗涤,之后合并有机层,柱色谱分离
2楼2010-09-20 16:16:33
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slowstar

木虫 (职业作家)

那一段合成的步骤,你应该拿得下来。
精韧不怠,日进有功
4楼2010-09-20 22:23:19
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