Reaction Steps
25 mmol of 5 are dissolved in 50 ml of THF and mixed with 25 mmol of NaH. After the termination of the evolution of hydrogen, 25 mmol of allyl bromide are added and the mixture is refluxed for 4 h. After cooling to room temperature, it is filtered off from the NaBr precipitation and the solvent is removed in a vacuum. A colorless oil remains. Yield: 98%. 1H NMR (400.1 MHz, 25° C., DMSO-d6): δ 7.80-7.25 (m, 14H, ar H, 5pz-H), 7.06 (t, 1H, 3JHH=6.6 Hz, 5-H), 6.63 (d, 1H, 3JHH=2.4 Hz, 4pz-H), 6.07-5.96 (m, 1H, —CH═CH2), 5.20-5.11 (m, 2H, —CH═CH2), 4.75 (d, 2H, 3JHH=5.7 Hz, —CH2CH═). 13C{1H} NMR (100.6 MHz, 25° C., DMSO-d6): δ 150.5 (C-3pz), 139.4 (C-5pz), 137.6 (d, 1JPC=12.0 Hz, C-1), 134.7 (—CH═CH2), 134.1 (d, 2JPC=19.4 Hz, C-o), 132.9 (d, 3JPC=2.8 Hz, C-3), 132.8 (d, 2JPC=14.8 Hz, C-6), 132.4 (d, 1JPC=9.2 Hz, C-1), 130.9 (d, 2JPC=25.0 Hz, C-2), 130.0 (d, 3JPC=4.6 Hz, C-5), 129.8 (s, C-p), 129.6 (d, 3JPC=6.5 Hz, C-m), 126.7 (s, C-4), 118.7 (—CH═CH2), 103.6 (C-4pz) 54.7 (—CH2CH═). 31P{1H} NMR (162.0 MHz, 25° C., DMSO-d6): δ 4.90.
