Reaktion #934712

Reaktionsgleichung

CO2

2'-methoxyacetophenone

O2

phenol

→

diphenyl carbonate

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe reactor is then flushed with 2×1500 psi CO
2. 2
   SonstigeThe reactor is flushed with 4×1500 psi O2
3. 3
   Sonstigeat the end of the fourth oxygen purge cycle
4. 4
   workup.ADDITIONThere is added to the oxygen atmosphere, 400 psi of CO2 and 900 psi of CO
5. 5
   Sonstigehas been produced

Vorschrift

There is charged 900 psi of CO2 into a reactor which is leak checked and then exhausted to atmospheric pressure. The reactor contains a mixture consisting of 50.0 g (0.531 mol) of phenol, 1.50 g (4.65 mmol) of TBAB, 0.55 g (0.245 mmol) of Pd(OAc)2, 0.040 g (0.226 mmol) of Co(OAc)2 and 0.340 g (2.02 mmol) of 2'-methoxyacetophenone. The reactor is then flushed with 2×1500 psi CO followed by pressurization to 2100 psi with CO (high pressure leak test) before exhausting it back to atmospheric pressure. The reactor is flushed with 4×1500 psi O2 ; at the end of the fourth oxygen purge cycle, the oxygen atmosphere in the reactor is reduced to 300 psig. There is added to the oxygen atmosphere, 400 psi of CO2 and 900 psi of CO. The reactor is heated to 100° C. Aliquots are taken at predetermined time to assess the amount of diphenylcarbonate which has been produced. After each sampling, the reactor atmosphere is rejuvenated by exhausting the atmosphere to 1000 psi (Pt), followed by the addition of 200 psi of O2 and 700 psi of CO. After 6 hours there is obtained 10.75% by weight of a red-brown diphenyl carbonate product.

Quelle