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qicaiju

铁杆木虫 (正式写手)

[求助] 有关氮丙啶中文文献翻译成英文(有效期至2011-5-16)

取42g硫酸酯,在冰水浴的冷却下向其中缓缓滴加12%的NaoH溶液180mL,同时用机械搅拌器搅拌,使白色固体完全溶解。在250mL三颈瓶中,加入14%的NaOH溶液10mL,加热至沸。通过滴液漏斗向其中滴加上述硫酸酯的碱溶液,106℃时溶液沸腾,开始有水和氮丙啶的混合液一起蒸出,接收瓶用冰盐浴冷却,冷凝器采用冰水冷凝。保持以较快的速度滴加,控制滴加速度与蒸出速度基本相等。加完后,再补加25mL蒸馏水。由于副产物Na2SO4。越来越多,逐渐积聚于瓶底,不仅容易暴沸,而且瓶中液体难以蒸完,因此待瓶中约剩余20mL溶液时,停止加热,将剩余液体转移至另一瓶中继续蒸馏。蒸馏完毕后,将馏出液转移至一装有机械搅拌器、温度计、两个冷凝管的四颈瓶中,在冰盐浴的冷却下,从一个冷凝管的上端向其中加入120g固体NaoH,使溶液温度保持在10℃以下,加完后,将液体转移至滴液漏斗中,分出上层氮丙啶液体,产量8.69,产率73%,将粗产品再用固体NaoH干燥几次后,对其进行分馏精制。收集b.p.56—57℃的馏份,再用金属Na干燥。
爱是一个长久的诺言,平淡的故事要用一生讲完~
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newtime007

木虫 (正式写手)

成长的微生物

【答案】应助回帖

qicaiju(金币+5, 博学EPI+1): 2011-05-15 18:18:48
Take 42g sulfuric acid ester, slowly drop 180mL NaoH solution with 12% into it with the mechanical agitator mixing using ice water bath cooling ,  make white solid completely dissolved. heat 10mL NaOH solution 14% in 250mL flask to a boiling,then drop sulfuric acid ester to above NaOH solution , water solution of the mixture with nitrogen c acetamiprid steamed out when heat to 106 ℃,receiving condensate with bottle in ice salt bath. control with steamed out speed and dropping speed equal , add again 25mL distilled water after end.Stop heating when surplus about 20mL solution in bottle, because Na2SO4 by-products,and gradually accumulate in bottle, not only easy in bottle, and critical boiling liquid hard to evaporate. Then the remaining liquid transferred to another bottle of continued distillation. Distillation finished, could metastasize to the distillate with mechanical agitator, a thermometer, two of the four neck flask condensing tubes in ice salt bath, the cooling condenser tubes from a top of the 120g solid NaoH joined to among them, make solution temperature below 10 ℃, remain in adds, will be transferred to the drops of liquid liquid nitrogen, cent gives hopper upper oxazolidine liquid, yield propylene yield 73% 869, coarse product, with solid NaoH dry again after a few times, and carry on the fractionation refined. Collect the b.p. 56-57 ℃, reoccupy metal fractions of making dry
上善若水,水善利万物而不争
2楼2011-05-15 14:48:41
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8023SH

金虫 (正式写手)

引用回帖:
1025456楼: Originally posted by qicaiju at 2011-05-12 20:49:18:
取42g硫酸酯,在冰水浴的冷却下向其中缓缓滴加12%的NaoH溶液180mL,同时用机械搅拌器搅拌,使白色固体完全溶解。在250mL三颈瓶中,加入14%的NaOH溶液10mL,加热至沸。通过滴液漏斗向其中滴加上述硫酸酯的碱溶液 ...

请问楼主,你的氮丙啶产率有73%吗?
3楼2012-04-21 13:56:34
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qicaiju

铁杆木虫 (正式写手)

引用回帖:
1553266楼: Originally posted by 8023SH at 2012-04-21 13:56:34:
请问楼主,你的氮丙啶产率有73%吗?

没有的,一次只能做出来6g左右。
爱是一个长久的诺言,平淡的故事要用一生讲完~
4楼2012-04-24 19:00:11
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8023SH

金虫 (正式写手)

引用回帖:
1554060楼: Originally posted by qicaiju at 2012-04-24 19:00:11:
没有的,一次只能做出来6g左右。

哦,我也做过,收率只有40%左右吧
5楼2012-04-24 22:43:21
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