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1460637084

铁虫 (小有名气)

[求助] Mechanism of formation of acetal 2

in a reaction flask(25ml) protected from moisture(CaCl2)solid MeONa (0.27g,5mmol)was suspended in DMF(4.5ml)at room temperature .A 1 M solution of CHCl3 in dmf (1ml)was dropped,over 1 min ,into the vigorously stirred suspension.the exothermic reaction raised the temperature to 36℃.after 30 min the reaction mixture was quickly poured into a volumetric flask(10ml).before diluting with DMF,n-nonane

Mechanism of formation of acetal 2
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818james

铜虫 (著名写手)

【答案】应助回帖

室温下,在一个用CaCl2隔绝湿气的反应瓶中, 将MeONa (0.27g,5mmol) 悬浮在DMF(4.5ml)中,缓慢滴加(用时超过1分钟)1ml氯仿dmf 液到剧烈搅动的悬浮液中。放热反应使唤液温上升到36℃。30分钟后将反应液迅速倾入10ml的容量瓶中。

后面的before diluting with DMF,n-nonane应属于另一句话了
3楼2016-09-29 11:33:29
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yqj89

专家顾问 (著名写手)

崇德瀹智

【答案】应助回帖

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1460637084(fjtony163代发): 金币+50, 代发 2016-10-26 00:10:33
fjtony163: 翻译EPI+1, 代发 2016-10-26 00:10:40
在一个25 ml隔绝水汽(就是插个CaCl2干燥管)的烧瓶中加入MeONa固体(0.27g,5mmol),并且在室温下用DMF(4.5ml)配成悬浊液(suspended)。

然后剧烈搅拌该悬浊液(vigorously stirred suspension),并用1min的时间缓慢滴加 1毫升 1M 的氯仿(CHCl3)DMF溶液。该放热反应(exothermic reaction)会把反应体系温度升高至36℃。

反应30 min之后,把反应体系(reaction mixture)快速倾倒至一个10mL定容瓶当中(volumetric flask),然后用DMF、n-nonane稀释
Now_or_Never
2楼2016-09-27 11:50:52
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