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【答案】应助回帖
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wangjieru: 金币+15, 翻译EPI+1, ★★★很有帮助 2013-04-21 11:41:23
Ethyl pyridine-2-carboxylate:
In 16L reactor, the 1170g of KMnO4 is dissolved into 16L water. And 100g 2-Picoline is chargedi into the solution. The oxidation reaction is exothermic and the reaction mixture is warmed. After the oxidation is finished, 225g 2-picoline is added carefully with good cooling system is necessary. After addition, another eauql quantity of 2-picoline(100 + 225 =325g) is added.
After the reaction is completed, the mixture is filtered, left ca.1/3 volume as cake, then washed with HCl:Congo acid(1:1), and then dried.
The syrup dired cake is heated to reflux in ethanol for 1 hour, filtered under hot condition. The filter cake is boiled in ethanol again and filtered under hot conditions. The mother liquor is concentrated, 440g of pyridine-2-carboxylic acid (51% yield, theoretical:859g) is obtained.
200g air dried crude product is dissolved into 340mL ethanol and added into 400mL Conc.H2SO4, heated to reflux for 4 hours. After reaction is finished, it is poured into 2kg ice, and adjusted to basic with 250g Na2CO3 and 500mL NH3 H2O.
The oil is separated and concentrated to produce 123g of ester (51% yield, theoretical: 245g).
Sdp.22 131-132℃ （This should be bp under vacuum） |
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