反応 #1956797

反応方程式

Tri-iso-butylphosphine

tributylphosphate

→

product

収率 68.5%

tri-iso-butyl-butylphosphonium dibutylphosphate

収率 68.5%

反応条件

後処理

1. 1
   workup.ADDITIONWhen the addition
2. 2
   workup.STIRRINGthe mixture was stirred at the same temperature for an additional 15 hours
3. 3
   温度The mixture was cooled down
4. 4
   その他moved to a rotary evaporator
5. 5
   その他dried under 160° C./5 mm Hg for 5 hours

実験手順

Tri-iso-butylphosphine (206.5 g, 98%, 1.0 mole) was added dropwise over a period of 2 hours to a flask containing 271.8 g (98%, 1.0 mole) of tributylphosphate at 200° C. under nitrogen and stirring. When the addition was complete, the mixture was stirred at the same temperature for an additional 15 hours. The mixture was cooled down and moved to a rotary evaporator and dried under 160° C./5 mm Hg for 5 hours. The product (320.7 g, yield 68.5%) was pure judged from NMR and liquid at room temperature. 1H-NMR (CDCl3, 300.13 MHz, δ): 3.76 (q, 4H, 2×CH3CH2CH2—CH2O—), 2.19 (q, 6H, 3×CH3 (CH3)CH—CH2P+), 1.96 (m, 3H, 3×CH3 (CH3)CH—CH2P+), 1.96 (m, 2H, CH3CH2CH2—CH2P+), 1.44 (m, 8H, CH3—CH2CH2—CH2O—), 1.24 (m, 4H, CH3—CH2CH2—CH2P+), 1.01 (d, 18H, 3×CH3CH(CH3)—CH2P+), 0.84 (t, 3H, CH3—CH2CH2CH2P+), 0.77 (t, 6H, 2×CH3—CH2CH2CH2O—). 31P-NMR (CDCl3, 81.015 MHz, δ): 32.60 (P+), −0.61 [d, (RO)2—P(═O)—O−].

出典