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2,3-Dichlorohexafluorobut-2-ene (E/Z isomer mixture) synthesis

12synthesis methods
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Yield:2418-21-5 17.9% ,2418-22-6 28.8%

Reaction Conditions:

with hydrogen at 170;Temperature;Reagent/catalyst;

Steps:

4 Example 4

Example 4 demonstrates the conversion of 11 3a to 131 6mxx over 2% Ru catalyst.An inconel tube (1/2 inch OD) was filled with 2 cc (1 .07 gm) of 2% Ru supported on 1/8” pellets either on SiC or CaE2. The temperature of the catalyst bed was raised to 120°C and purged with hydrogen (50 sccm) for 60 minutes and then at 250°C for 180 minutes. The temperature wasthen lowered to 175°C for 120 minutes while maintaining a hydrogen flowof 20 sccm. The temperature was lowered to 160°C and the flow of CEC19 1 13a (CF300I3) set to 2.31 mI/hour and the hydrogen to 32 sccm. The reactor effluent was analyzed every hour via online GCMS and then the results averaged to give the values in the table below. The temperature was raised to 17000 and the effluent analyzed every hour for four hours,averaged, and shown in the table below.

References:

WO2015/120250,2015,A1 Location in patent:Page/Page column 19; 20