Study on synthesis technology of bis(4-Nitrophenyl) carbonate by the triphosgene method

In this paper,synthesis technology of bis(4-nitrophenyl) carbonate(BPNPC) using bis(trichloromethyl) carbonate(BTC) with 4-Nitrophenol(PNP) was optimized.Effects of reaction temperature,catalyzator and feed ratio on synthesis of the product were investigated.The chemical structure of the product was characterized by means of the melting point and IR.The results show that tetraethylammonium bromide which was used as a phase transfer catalyst in this reaction had optimization effect on the interfacial diffusive reaction of BTC and PNP.Higher concentration of sodium hydroxide,lower temperature and a higher dosage of BTC produced a small amount of 4-nitrophenyl chloroformate,while lower concentration of sodium hydroxide and a lower dosage of BTC made reaction incomplete,which affected the yield.Optimal conditions for preparation of BPNPC were as follows: recoverable dichloromethane with low toxicity was used as the solvent,tetraethylammonium bromide was added at 25 ℃,n(BTC)∶n(NaOH)∶n(PNP)=1.0:1.05:6.4,and the sodium hydroxide concentration was 17%,and thus the highest yield could reach 95.2%.