Preparation method of multi-branched dicarboxylic ammonium salt and application thereof
A dicarboxylic acid, multi-branched technology, applied in the preparation of carboxylate, carboxylate/lactone, and sulfonate, etc., can solve the problem of high raw material cost, long carbon chain straight-chain tetracarboxylate, etc. It is not easy to obtain and other problems, and achieves the effects of low cost, novel process route and high yield.
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Embodiment 1
[0038] This embodiment discloses a kind of preparation method of polybranched dibasic carboxylic acid ammonium salt, comprises the following steps:
[0039] 1) Add 200 g of acetonitrile and 90.0 g of 1,4-butanediol into a four-neck flask with a volume of 2 L that is fully dried and equipped with stirring, dropping funnel, and thermometer, cool down to 0 ° C, and then add Slowly add a mixture of 381.4 g of p-toluenesulfonyl chloride and 400 g of acetonitrile dropwise. After the dropwise addition, keep the temperature at 0-5°C and continue stirring for 3 hours;
[0040] 2) Add 160.2 g of diethyl malonate and 106.0 g of sodium carbonate to the flask in step 1), heat up to 80° C., reflux for 3 hours, distill off acetonitrile, add water to separate the organic layer;
[0041] 3) Add 200 g of acetonitrile and 46.1 g of ethanol into a fully dried four-neck flask with a volume of 2 L and a stirring, dropping funnel, and thermometer, cool down to 0° C., and slowly add p-methyl A mixtu...
Embodiment 2
[0046] This embodiment discloses a kind of preparation method of polybranched dibasic carboxylic acid ammonium salt, comprises the following steps:
[0047] 1) Add 200 g of acetonitrile and 90.0 g of 1,4-butanediol into a four-neck flask with a volume of 2 L that is fully dried and equipped with stirring, dropping funnel, and thermometer, cool down to 0 ° C, and then add Slowly add a mixture of 381.4 g of p-toluenesulfonyl chloride and 400 g of acetonitrile dropwise. After the dropwise addition, keep the temperature at 0-5°C and continue stirring for 3 hours;
[0048] 2) Add 160.2 g of diethyl malonate and 106.0 g of sodium carbonate to the flask in step 1), heat up to 80° C., reflux for 3 hours, distill off acetonitrile, add water to separate the organic layer;
[0049] 3) Add 200 g of acetonitrile and 60.1 g of n-propanol into a fully dried four-neck flask with a volume of 2 L and a stirring, dropping funnel, and thermometer, cool down to 0° C., and slowly add the A mixture...
Embodiment 3
[0054] This embodiment discloses a kind of preparation method of polybranched dibasic carboxylic acid ammonium salt, comprises the following steps:
[0055] 1) Add 200 g of acetonitrile and 90.0 g of 1,4-butanediol into a four-neck flask with a volume of 2 L that is fully dried and equipped with stirring, dropping funnel, and thermometer, cool down to 0 ° C, and then add Slowly add a mixture of 381.4 g of p-toluenesulfonyl chloride and 400 g of acetonitrile dropwise. After the dropwise addition, keep the temperature at 0-5°C and continue stirring for 3 hours;
[0056] 2) Add 160.2 g of diethyl malonate and 106.0 g of sodium carbonate to the flask in step 1), heat up to 80° C., reflux for 3 hours, distill off acetonitrile, add water to separate the organic layer;
[0057] 3) Add 200 g of acetonitrile and 74.1 g of n-butanol into a four-neck flask with a volume of 2 L that is fully dried and equipped with stirring, dropping funnel, and thermometer, cool down to 0° C., and slowly...
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