Preparation method of 2,3,4,5-tetrafluorobenzoyl chloride

Preparation method of 2,3,4,5-tetrafluorobenzoyl chloride

  • CN 102,603,521 B
  • Filed: 02/09/2012
  • Issued: 03/04/2015
  • Est. Priority Date: 02/09/2012
  • Status: Active Grant
First Claim
Patent Images

1. the preparation method of a phenyl tetrafluoride formyl chloride, is characterized in that, comprises the following steps:

  • with 3,4,5,6-ptfe phthalate for raw material, in aromatic hydrocarbon solvent, under catalyzer organic tertiary amine exists, in 120 ~ 160 odecarboxylic reaction 10 ~ 30 hours under C, after reacting completely, reaction system is cooled to 20 ~ 30 oc, filters, and filtrate cover is used for lower batch of decarboxylic reaction, leach 2,3,4, chloride reagent and organic amide class catalyzer is directly added, temperature reaction 3 ~ 15 hours, after acyl chloride reaction is complete in 5-tetrafluorobenzoic aid solid, reaction system is steamed except low-boiling-point substance, through rectification under vacuum, obtain 2,3,4,5-phenyl tetrafluoride formyl chloride finished product;

    In described decarboxylic reaction, react when being less than 1% to 3,4,5,6-ptfe phthalate content, reaction system is cooled to 20 ~ 30 oc;

    Described aromatic hydrocarbon solvent be toluene, dimethylbenzene, trimethylbenzene, chlorobenzene any one or a few, solvent load is 1 ~ 20 times of 3,4,5,6-ptfe phthalate quality;

    Described organic tertiary amine is selected from Tri-n-Propylamine, tri-isopropyl amine, diisopropyl ethyl amine, tri-n-butylamine, N-methylmorpholine, N, any one or a few of N-lupetazin, N-crassitude, organic tertiary amine and 3,4, the ratio of 5,6-ptfe phthalate amount of substance is 0.005;

    1 ~ 0.2;

    1;

    Described chloride reagent be selected from sulfur oxychloride, two (trichloromethyl) carbonic ether one or both, chloride reagent is 0.33;

    1 ~ 10;

    1 with the ratio of the amount of substance of 2,3,4,5 tetra fluoro benzoic acid;

    Described organic amide class catalyzer is selected from N, dinethylformamide, N, one or more of the 1-N-piperazinyl-4-formaldehyde that N-diethylformamide, N-formyl piperidine, N-formyl morpholine, Merrifield are resin-carried, organic amide class catalyzer and 2,3, the ratio of the amount of substance of 4,5-tetrafluorobenzoic aid is 0.01;

    1 ~ 0.1;

    1;

    Described acyl chloride reaction carries out under solvent environment, solvent be selected from trichloromethane, ethylene dichloride, toluene, dimethylbenzene, trimethylbenzene, chlorobenzene one or more, solvent load is 1 ~ 10 times of 2,3,4,5 tetra fluoro benzoic acid quality.

View all claims
    ×
    ×

    Thank you for your feedback

    ×
    ×