反应详情

Triethylphosphine (7.2 g, 99%, 0.06 mol) was added dropwise to a 125 mL flask containing 12.6 (99%, 0.06 mol) di-n-butylsulfate at 80° C. under nitrogen and with stirring over a period of 75 minutes. The liquid was stirred at 140° C. for an additional 3.5 hours. The liquid was cooled, moved to a rotary evaporator and dried at 125° C./5 mm Hg for 6 hours. The product (16.73 g, yield 85%) was a wax-like solid at room temperature (m.p. from DSC measurement: 40.0° C.). 1H-NMR (CDCl3, 300.13 MHz, δ): 3.98 (t, 2H, CH3CH2CH2—CH2—O—), 2.34 (m, 8H, 3×CH3—CH2P+ and CH3CH2CH2—CH2P+), 1.54 (m, 8H, CH3—CH2CH2—CH2O— and CH3—CH2CH2—CH2P+), 1.25 (m, 3×CH3—CH2P+), 0.91 (m, 6H, CH3CH2CH2—CH2O— and CH3CH2CH2—CH2P+). 31P-NMR (CDCl31 81.015 MHz, δ): 38.88 (s, P+).

1. stirringThe liquid was stirred at 140° C. for an additional 3.5 hours
2. temperatureThe liquid was cooled
3. custommoved to a rotary evaporator
4. customdried at 125° C./5 mm Hg for 6 hours