反应详情

温度

210 °C

Ph2P(CH2)3P(H)Ph (3.68 g, 10.9 mmol), allyldiethylphosphine (1.71 g, 13.1 mmol) and AIBN (0.011 g) were mixed in a Schlenk flask and radiated with a 365 nm UV lamp for 20 hours. After confirming that the reaction was complete by 31P NMR analysis, it was distilled under vacuum (<0.5 mm Hg) at a final heating mantle temperature of 210° C. for an hour to remove impurities. The ligand remained in the pot. Yield: 3.36 g (66%). 31P NMR (122 MHz, CDCl3, δ, ppm): −16.74 (s), −23.09 (s) and −25.98 (s). There are peaks near the three major peaks, which have not been determined if are part of the ligand or due to impurities. 1H NMR (500 MHz, CDCl3, δ, ppm): 1.001 (d of q, JH-P&H=7.0 Hz 4H's methylenes of ethyl groups), 1.3 to 2.2 (m, H's on methyls and propylenes) (d of t, JH-P&H=211 & 6.6 Hz, H on the P), and 7.30 to 7.47 (m, 15H's on phenyl rings).

1. distillationwas distilled under vacuum (<0.5 mm Hg) at
2. customto remove impurities