4H-OCTAFLUORO-1-IODOBUTANE synthesis
- Product Name:4H-OCTAFLUORO-1-IODOBUTANE
- CAS Number:754-73-4
- Molecular formula:C4HF8I
- Molecular Weight:327.94
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Yield:-
Reaction Conditions:
with N,N-dimethyl-formamide;zinc in 5,5-dimethyl-1,3-cyclohexadiene at -78 - 140;Reagent/catalyst;
Steps:
9 Example 2: ClCF2-CFCl-CF2-CF2I; post-additional; no iodine-containing inorganic material
General procedure: 200 g (0.53 mol) of xylene and 34.93 g (0.53 mol) of zinc were added to an eggplant flask with a condenser connected with a trap cooled to -78 ° C., and heated under stirring until the internal temperature was 140 ° C. After the inner temperature became constant, N, N-dimethylformamide (DMF) was added dropwise for 1 hour at a dripping rate of 0.52 mol / hour (1.04 mol / hour with respect to 1 mol of zinc) while refluxing, and heatingrefluxwas continued for 0.5 hours while stirring. Then, while refluxing, the raw material (ClCF 2-CFCl-CF2-CF2I) was added dropwise at a dripping rate of 0.24 mol / hour (0.48 mol / hour for 1 mol of zinc) for 1 hour, and the reaction was continued by heatingrefluxfor 3 hours while stirring. After the completion of the reaction, the gas phase, liquid phase, and reaction liquid of the collection cylinder were analyzed by gas chromatomography, and the conversion rate and selectivity were calculated in consideration of each, and the conversion rate was 100 mol%, and the selectivity of each component was CF 2 = CFCF = CF 2 78 mol%, CF 2 = CF-CF2-CF2H is 14 mol%, ClCF 2-CFCl-CF = CF 2 is 0.66 mol%, ClCF 2-CFCl-CF2-CF2 H is 1.5 mol%, and other by-products (CF3CF = CHCF3etc.) for a total of 5.9 mol%.
References:
JP2023/21141,2023,A Location in patent:Paragraph 0046; 0053; 0061
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