Phenol → HCID 86610182, compound

Temperature

67.5 °C

Phenol (331 g, 3.525 moles) was placed in a three neck round bottom flask equipped with a mechanical stirrer, a vacuum/gas port and an addition funnel and heated to 65-70° C. under nitrogen. Phosphorous trichloride (137.3 g, 1.0 mole) was added to the heat phenol dropwise via the addition funnel over a three hour period under nitrogen. Following the complete addition of the phosphorous trichloride, the reaction mixture was stirred at 70° C. for an additional hour. The temperature was then increased to 250° C. under nitrogen until all of the excess phenol had distilled off. The reaction mixture was allowed to cool to room temperature under nitrogen. The next day the temperature was raised to 260° C. and methanol was slowly added. During the addition of methanol the temperature varied from 260° C. to 204° C. After the methanol addition was complete, the reaction temperature was maintained between 210° C. to 215° C. and the reaction was stirred. An aliquot was removed and analyzed by gas chromatography (GC) every hour until no trace of triphenylphosphite could be detected. After 1 hour, the GC analysis indicated that 2.031% triphenylphosphite remained in the reaction mixture. After 2 hours, no triphenylphosphite was detected by GC.

1. customequipped with a mechanical stirrer
2. distillationhad distilled off
3. temperatureto cool to room temperature under nitrogen
4. temperatureThe next day the temperature was raised to 260° C.
5. additionmethanol was slowly added
6. additionDuring the addition of methanol the temperature
7. customvaried from 260° C. to 204° C
8. additionAfter the methanol addition
9. temperaturethe reaction temperature was maintained between 210° C. to 215° C.
10. stirringthe reaction was stirred
11. customAn aliquot was removed
12. waitanalyzed by gas chromatography (GC) every hour until no trace of triphenylphosphite
13. waitAfter 2 hours

ORD record

ord-2d46642cd4f240f580f022439592387b

Source dataset

uspto-grants-2009_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07569717B2