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Тема |
Re: Тук: [re: devilme] |
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Автор |
id2578 (непознат
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Публикувано | 18.11.08 22:51 |
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Аз намерих това:
Preparation of Ac2O from thionylchloride was successful, here is description of my experiment:
120 ml of glacial acetic acid was added to 144 ml of thionylchloride, reaction takes place on mixing, leading to formation of HCl+SO2 and mixture is strongly cooled (endotermic reaction). Mixture is allowed to stand at room temperature for 2 hours, allowing most of HCl and SO2 to evolve. Next, reaction mixture is placed on water bath under efficent reflux condenser, tubing was tightly attached to end of condenser to vent reaction gasses to outside, bath was heated to 55C and mixture is left at this temperature for 2 hours. During this period convertion of acetic acid to acetylchloride is fully completed, and gas evolution ceases. Reaction product was cooled to room temperature and then in ice bath, 160g of freshly melted pulverized sodium acetate was added with stirring. Addition rate is adjusted, to not allow reaction mixture to boil. After acetate is added mixture is allowed to stand for 30 minutes at room temperature and was destilled. All liquid phase from reaction mixture is distilled off in temperature interval about 4C (about 136-140C), about 200 ml of distillate is obtained witch is acetic anhydride. Yield was not precisely mesasured but it is close to that predicted by theory. Reaction equations:
SOCl2 + CH3COOH => CH3COCl + HCl + SO2
СH3COCl + CH3COONa => (CH3CO)2O + NaCl
Дано помогне...
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