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16034-43-8

P-XYLENE-2,3,5,6-D4 synthesis

2synthesis methods
-

Yield:1603-99-2 72 % ,62367-40-2 4 % ,16034-43-8 4 %

Reaction Conditions:

with aluminum chlorofluoride;tri-n-butyl-tin hydride in benzene-d6 at 70;Schlenk technique;

Steps:

Dehydrofluorination of 1,1-difluoroethane at ACF in the presence of HSnBu3

A reaction of 1,1-difluoroethane (0.26 mmol) in C6D6 gave after 7 days 1- fluoroethylene with a yield of 48%. NMR data of 1-fluoroethylene[19]: 1H NMR (300 MHz, C6D6): δ= 6.10 (ddd, 1H, =CFH, 2JH,F= 85 Hz, 3JH,H= 13, 3JH,H= 5 Hz), 4.52 (ddd, 1H, CF=CH, cis-CH, 3JH,F= 20 Hz, 3JH,H=13, 2JH,H=3 Hz), 3.95 (ddd, 1H, trans-CHF, 3JH,F= 53, 3JH,H=5, 2JH,H=3 Hz) ppm. 19F NMR (282 MHz, C6D6): δ= 115.0 (ddd, 1F, CHF, 2JF,H = 85, 3JF,H= 53, 3JF,H= 20 Hz) ppm

References:

Pan, Xinzi;Talavera, Maria;Braun, Thomas [Journal of Fluorine Chemistry,2022,vol. 263,art. no. 110046] Location in patent:supporting information

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