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ChemicalBook CAS DataBase List o-[1-(4-hydroxyphenyl)-1-methylethyl]phenol

o-[1-(4-hydroxyphenyl)-1-methylethyl]phenol synthesis

7synthesis methods
-

Yield: 63.2% , 11.43% , 0.01%

Reaction Conditions:

beta zeolite acidic form at 120; under 760.051 Torr; for 12 h;

Steps:

2 EXAMPLE 2-SYNTHESIS OF BISPHENOL A WITH BETA ZEOLITE Bath test at atmospheric pressure
EXAMPLE 2-SYNTHESIS OF BISPHENOL A WITH BETA ZEOLITE Bath test at atmospheric pressure 9.4 g of phenol (0.1 moles) and 1.16 g of acetone (0.02 moles) with a phenol/acetone molar ratio of 5/1, and 1 g of beta zeolite prepared according to example 1, are charged into a glass flask, equipped with a stirrer and water cooler, immersed in a thermostat-regulated oil bath. The above suspension is maintained under stirring for 12 hours, at atmospheric pressure (1 atm), with a bath temperature of 120C. At the end the mass is cooled down to room tempera- ture. The reaction product is analyzed by means of HPLC, with the analysis method described in Journal fur Prak- tische Chemie, Band 328, Heft 1,1986, pp. 142-148. Acetone conversion: 99. 9% Selectivity to p, p'bisphenol A: 63. 20% Selectivity to o, p'bisphenol A: 16. 54% Selectivity to trimers and heavy products: 20.14% Selectivity to mesityl oxide (undesired by-product) lower than the analytical limit (0.01%). EXAMPLE 3-SYNTHESIS OF BISPHENOL A WITH BETA ZEOLITE Bath test, at atmospheric pressure with extraction in continuous of the water formed 9.4 g of phenol (0. 1 moles) and 1.16 g of acetone (0.02 moles) with a phenol/acetone molar ratio of 5/1, and 1 g of beta zeolite prepared according to example 1, are charged into a glass flask, equipped with a stirrer and Dean-Stark trap with a water cooler, immersed in a thermostat-regulated oil bath. The suspension described above is maintained under stirring for 6 hours with a bath temperature of 120C. The system is at atmospheric pressure (1 atmosphere). The toluene-water azeotropic mixture formed during the reaction is continuously removed by means of the Dean- Stark trap. Said azeotropic mixture demixes at room tem- perature: the aqueous phase is removed, whereas toluene is re-fed to the flask. At the end the mass is cooled down to room tempera- ture. The reaction product is analyzed by means of HPLC, with the analysis method described in Journal fur Prak- tische Chemie, Band 328, Heft 1,1986, pp. 142-148. Acetone conversion: 99. 9% Selectivity to p, p'bisphenol A: 72. 31% Selectivity to o, p'bisphenol A: 11. 43% Selectivity to trimers and heavy products: 16.16% Selectivity to mesityl oxide (undesired by-product) lower than the analytical limit (0. 01%).

References:

ENITECNOLOGIE S.P.A. WO2004/48302, 2004, A1 Location in patent:Page 21-22