反応 #53631

反応方程式

octanol

phosphorus trichloride

phosphorus-31

octanol

→

Octylphosphorodichloridite

反応条件

後処理

1. 1
   その他equipped with a mechanical stirrer, an addition funnel
2. 2
   その他a thermometer, and a reflux condenser itself topped with a discharge tube
3. 3
   その他The discharge tube led to an aqueous sodium hydroxide trap for absorption of hydrogen chloride that
4. 4
   その他evolves from the reaction
5. 5
   workup.ADDITIONwas added dropwise to the reaction mixture
6. 6
   温度to warm gradually up to room temperature
7. 7
   workup.ADDITIONwas then poured into a dry distillation flask
8. 8
   workup.DISTILLATIONThe material was distilled with a bath temperature of 80-85° C.
9. 9
   その他to remove residual hydrogen chloride and excess phosphorus trichloride
10. 10
    その他to yield the product at 113-130° C. in 69% conversion
11. 11
    その他at 21.5° C.

実験手順

Freshly distilled phosphorus trichloride (45.6 g, 0.338 mole) was charged into a four-necked round bottom flask equipped with a mechanical stirrer, an addition funnel, a thermometer, and a reflux condenser itself topped with a discharge tube. The discharge tube led to an aqueous sodium hydroxide trap for absorption of hydrogen chloride that evolves from the reaction. After cooling the reaction vessel to 0° C. with continual purging of dry nitrogen, anhydrous octanol (22 g, 0.168 mole) was added dropwise to the reaction mixture. When the addition of the octanol was complete, the reaction mixture was allowed to warm gradually up to room temperature and was then poured into a dry distillation flask. The material was distilled with a bath temperature of 80-85° C. and using a water pump vacuum to remove residual hydrogen chloride and excess phosphorus trichloride. The residue was then fractionated at 8 mm Hg to yield the product at 113-130° C. in 69% conversion. The phosphorus-31 NMR showed a peak at 176 ppm. The refractive index at 21.5° C. was 1.4682.

出典