4-fluoro-5-oxo-2,4-bis(trifluoromethyl)-1,3-dioxolane-2-carbonyl fluoride synthesis

4synthesis methods

Product Name:4-fluoro-5-oxo-2,4-bis(trifluoromethyl)-1,3-dioxolane-2-carbonyl fluoride
CAS Number:7345-49-5
Molecular formula:C6F8O4
Molecular Weight:288.05

428-59-1 Synthesis

428-59-1
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4-fluoro-5-oxo-2,4-bis(trifluoromethyl)-1,3-dioxolane-2-carbonyl fluoride

7345-49-5
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$95.00/1 g

Yield: 86%

Reaction Conditions:

with 4-methoxy-benzaldehyde at 85 - 140; under 1500.15 - 5250.53 Torr; for 19 h;Autoclave;Large scale;Temperature;Reagent/catalyst;Pressure;

Steps:

1; 2; 3; 4; 5; 6; 7; 8; 9; 10; 11; 12; 13; 14; 15; 16; 17; 1 Example 15 Preparation of trifluoropyruvic acid fluoride dimer
Using the same reactor as in Example 1, 4-methoxybenzaldehyde (2.38 kg, 17.48 mol) was charged and heated to 85 ° C., while maintaining the same temperature, hexafluoropropylene oxide (3.15 kg, 18.1 mol). 97 mol) was continuously supplied over 7 hours to carry out the reaction step.The pressure during this period was a maximum of 0.2 MPa. Next, the reaction was performed at a reaction temperature of 140 ° C. for 12 hours. The maximum pressure at 140 ° C. was 0.7 MPa.After completion of the reaction, the mixture was cooled to room temperature and then separated to obtain a crude trifluoropyruvic acid dimer (light yellow transparent liquid, 2.35 kg).In the quantification by 19F-NMR using benzotrifluoride as an internal standard,2.17 kg (7.53 mol) of the desired product, trifluoropyruvic acid dimer, was produced (86% yield, based on 4-methoxybenzaldehyde).

References:

Tosoh Corporation;Tosoh Finechem Corporation;Miyauchi, Hideki;Matsuo, Hiroshi;Kagawa, Takumi;Kondo, Norihisa JP2020/37548, 2020, A Location in patent:Paragraph 0027-0050; 0052