Trifluoroacetic anhydride synthesis

10synthesis methods

Product Name:Trifluoroacetic anhydride
CAS Number:407-25-0
Molecular formula:C4F6O3
Molecular Weight:210.03

Trifluoroacetic anhydride is prepared by reaction of trifluoroacetyl chloride with an alkali metal or alkaline-earth metal salt of trifluoroacetic acid at approximately 50° C.

76-05-1 Synthesis

76-05-1
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407-25-0
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Yield:407-25-0 99%

Reaction Conditions:

with fuming sulphuric acid at 130;Large scale;

Steps:

Production of trifluoroacetic anhydride

A 115 1 ceramic-lined Pfaundler stirred vessel equipped with a 2.5 m packing column filled with 10 mm glass Raschig rings and equipped with a condenser was filled with 70.5 kg trifluoroacetic acid followed by 19.1 1 65 % oleum, i.e. oleum with 65 wt % free S03. Subsequently, the Pfaundler vessel was heated by means of an oil bath to a temperature of 130 °C. The product was removed by distillation at a rate of 7.4 kg/h and directed into PE-lined metal drums. During the distillation the temperature of the reaction mixture changed gradually from 78 °C to 96 °C. The yield of trifluoroacetic anhydride was 64.9 kg (99 %). The purity of the product was > 99.9 %. Additionally, 7.8 kg of a tailing fraction was obtained that contained trifluoroacetic anhydride and trifluoroacetic acid next to other not identified side products. This second fraction can be submitted to the reaction mixture of a subsequent batch.

References:

WO2014/195929,2014,A2 Location in patent:Page/Page column 4