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ChemicalBook CAS DataBase List enbucrilate
6606-65-1

enbucrilate synthesis

6synthesis methods
-

Yield:6606-65-1 440 g

Reaction Conditions:

with phosphoric acid;sulfuric acid;toluene-4-sulfonic acid;acetic acid;chloroacetic acid at 100 - 115;Reagent/catalyst;Temperature;

Steps:

2; 3; 4; 5; 7; 8; 9; 10 Preparation method of n-butyl cyanoacrylate:
500 g of the α-cyanoacrylate ethyl ester monomer prepared in Example 1 was placed in a 1000 ml flask, and a mixture of 2% glacial acetic acid and anhydrous phosphoric acid (the molar ratio of glacial acetic acid to anhydrous phosphoric acid was 0.7:1) was added. 0.35% of hydroquinone and 0.45% of a mixture of concentrated sulfuric acid and p-toluenesulfonic acid (the molar ratio of concentrated sulfuric acid to p-toluenesulfonic acid is 1:1), adding 444 g of n-butanol, stirring and heating, controlling the pot temperature of 100 -115 ° C, collect the ethanol fraction of the top of 76-82 ° C; increase the temperature of the kettle to 120-140 ° C, normal pressure and pump decompression (-0.1MPa) to collect n-butanol, oil pump decompression (200-800Pa) Fractions with >98% content were collected until the temperature at the top of the column decreased significantly. 440 g of n-butyl cyanoacrylate having a content of >99% was obtained.

References:

Hebei Chengxin Group Co., Ltd.;Wang Hong;Li Chengguo;Zhang Chaochun;Fan Chunyan;Sun Jiehao;Liu Shaojun;Dong Jin CN109810021, 2019, A Location in patent:Paragraph 0061; 0062; 0063; 0064; 0065; 0066; 0067-0085

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