反应详情

温度

200 °C

Tri-n-butylphosphine (215 g, 94%, 1.0 mole) was added dropwise over a period of 4 hours to a flask containing 272 g (98%, 1.0 mole) of tributylphosphate at 170° C. When the addition was complete, the reaction mixture was heated to 200° C. and stirred at this temperature for 24 hours. The viscous liquid was dried in a rotary evaporator at 160° C./5 mm Hg for 5 hours. The product (363 g, yield 77.5%) was pure according to NMR. At room temperature the product was a white, wax-like solid (m.p. from DSC measurement: 28.0° C.). 1H-NMR (CDCl3, 300.13 MHz, δ): 3.84 (q, 4H, 2×CH3CH2CH2—CH2—O—), 2.38 (m, 8H, 4×CH3CH2CH2—CH2P+), 1.53 (m, 16H, 4×CH3—CH2CH2—CH2P+), 1.40 (m, 8H, 2×CH3—CH2CH2—CH2O—), 0.97 (m, 12H, 4×CH3—CH2CH2CH2P+), 0.90 (m, 6H, 2×CH3—CH2CH2CH2O—). 31P-NMR (CDCl3, 81.015 MHz, δ): 33.72 (P+), 0.94 [m, (RO)2—P(═O)—O−].

1. additionWhen the addition
2. customThe viscous liquid was dried in a rotary evaporator at 160° C./5 mm Hg for 5 hours