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ChemicalBook CAS DataBase List Pentaerythritol tetrakis(2-mercaptoacetate)

Pentaerythritol tetrakis(2-mercaptoacetate) synthesis

3synthesis methods
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Yield:10193-99-4 76 %Chromat.

Reaction Conditions:

with toluene-4-sulfonic acid in toluene at 130; for 9 h;Dean-Stark;Inert atmosphere;

Steps:

1 Synthesis Example 1: Preparation of a polythiol compound
Install a mechanical stirrer, Dean Stark device with one of the cooling pipes, A thermometer connected to a temperature controller, And one of the reactors was charged with 187.5 grams (2.04 moles) of thioglycolic acid, 63.0 grams (0.46 moles) of pentaerythritol, 0.8 g of p-toluenesulfonic acid and 469.0 g of toluene. The mixture was stirred for 60 minutes, and then reacted at 130 ° C for 8 hours. In this case, a nitrogen tube is installed inside the reactor, and nitrogen is continuously supplied through the nitrogen tube to remove water generated during the reaction in the reactor, thereby inducing the reaction to be positive. Here, the amount of water removed is 98.9% of the theoretical amount. Then, the temperature was lowered to room temperature, and then, an organic layer was obtained by performing sequential alkaline cleaning and water cleaning. The organic layer thus obtained was heated and decompressed to remove the solvent. It was then cooled to room temperature and filtered to obtain 199.5 g of a polythiol composition containing a compound represented by Chemical Formula 4 as a main component. The polythiol composition thus obtained is subjected to an absolute calibration method, A liquid chromatography (Shimadzu, Nexera SR, detector: photodiode array (PDA)) was used to analyze and quantify the compounds contained in the composition. Therefore, the thus obtained polythiol composition contains 76% by weight of the polythiol compound represented by Chemical Formula 4, 2% by weight of a polythiol compound represented by Chemical Formula 6, And 22% by weight of oligomer compounds other than the compounds of Chemical Formulas 4 and 6.

References:

SKC CO., LTD.;SHIM, JONGMIN;HONG, SEUNG MO;SEO, HYEON MYEONG;SHIN, JUNGHWAN TW2019/30263, 2019, A Location in patent:Paragraph 0061; 0062

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