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newtime007

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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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