تفاعل #53631

معادلة التفاعل

octanol

phosphorus trichloride

phosphorus-31

octanol

→

Octylphosphorodichloridite

ظروف التفاعل

المعالجة

1. 1
   أخرىequipped with a mechanical stirrer, an addition funnel
2. 2
   أخرىa thermometer, and a reflux condenser itself topped with a discharge tube
3. 3
   أخرىThe discharge tube led to an aqueous sodium hydroxide trap for absorption of hydrogen chloride that
4. 4
   أخرىevolves from the reaction
5. 5
   workup.ADDITIONwas added dropwise to the reaction mixture
6. 6
   درجة الحرارةto 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
   أخرىto remove residual hydrogen chloride and excess phosphorus trichloride
10. 10
    أخرىto yield the product at 113-130° C. in 69% conversion
11. 11
    أخرىat 21.5° C.

الإجراء التجريبي

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.

المصدر