تفاعل #79451

معادلة التفاعل

KOH

BPA

phenyldichlorophosphate

aluminum chloride

phenol

→

BPA phosphate

المردود 91.0%

ظروف التفاعل

المعالجة

1. 1
   أخرىfitted with an overhead stirrer, a water condenser with nitrogen outlet and a nitrogen inlet
2. 2
   أخرىto absorb the evolved HCl
3. 3
   workup.WAITleft
4. 4
   درجة الحرارةthe temperature was increased to 140° C.
5. 5
   workup.STIRRINGstirred at that temperature for 4 hours
6. 6
   workup.WAITwas applied at 120° C. for 2 hours
7. 7
   أخرىto remove excess phenol
8. 8
   درجة الحرارةThe temperature was further increased to 140° C.
9. 9
   workup.WAITto a maximum for 180° C. and the reaction mixture was held under vacuum for additional 4 hours
10. 10
    workup.ADDITIONThe reaction mixture was poured while it

الإجراء التجريبي

24.81 g (0.11 mol) of BPA, 25.00 g (0.12 mol) of phenyldichlorophosphate, and 0.22 g (1.64 mmol) of aluminum chloride were taken in a cylindrical glass reactor fitted with an overhead stirrer, a water condenser with nitrogen outlet and a nitrogen inlet. The nitrogen outlet was immersed in a beaker containing KOH solution to absorb the evolved HCl. The reaction mixture was stirred at 90° C. for 2 hours and further at 120° C. for 4 hours. A sample of the reaction mixture was drawn and 31P NMR spectrum was done to show that there was no phenyidichlorophosphate left; the conversion was nearly 75%. To the reaction mixture 4.49 g (0.05 mol) of phenol was added and the temperature was increased to 140° C. and stirred at that temperature for 4 hours. After confirming from the 31P NMR spectrum that there were no reactive P—Cl bonds, vacuum (0.01 mm Hg) was applied at 120° C. for 2 hours to remove excess phenol. The temperature was further increased to 140° C. and then to a maximum for 180° C. and the reaction mixture was held under vacuum for additional 4 hours. The reaction mixture was poured while it was in molten state onto aluminum foil to afford 36 g (yield ˜91%) a straw yellow, transparent solid poly-(BPA-phosphate).

المصدر