4-Chloroformylphthalic anhydride synthesis

Yield:1204-28-0 150.6 g

Reaction Conditions:

with thionyl chloride;tributylphosphine in ethyl acetate at 80; for 6 h;Solvent;Temperature;

Steps:

1
200 g of trimellitic anhydride, 120 mL of ethyl acetate and 0.02 g of tri-n-butylphosphine were added to the reaction flask, and the temperature was raised to 80 ° C.156 g of thionyl chloride was slowly added dropwise, and the reaction was refluxed for 6 hours until no gas evolved, and the reaction was completed to obtain a reaction solution.The reaction solution was distilled at -0.085 MPa at 80 ° C to recover residual benzene and excess thionyl chloride, and then vacuum distilled through a thin film evaporator.The degree of vacuum was 660 mmHg and the temperature was 130 °C.Collect 180-190 ° C fractions,Obtained 150.6 g of trimellitic anhydride acid chloride,After cooling, it was a white solid crystal with a melting point of 68.1 ° C and an HPLC chromatographic content of 99.25%.

References:

Shandong Kaisheng New Materials Co., Ltd.;Xue Juqiang;Zhang Congcong;Huang Guiqing;Zhang Taiming;Wang Ronghai;Han Nannan;Wang Jun;Li Guanghui;Sun Qingmin;Zhang Jiliang;Shi Yufei CN108341796, 2018, A Location in patent:Paragraph 0016; 0017; 0018; 0019; 0020; 0021