反応 #59231

反応方程式

bisphenol A

phosgene

sodium hydroxide

p-tert.-butylphenol

sodium hydroxide

n-ethylpiperidine

4,4′-dihydroxydiphenyl ether

→

bisphenol A 4,4′-dihydroxydiphenyl ether

溶媒

methylene chloride

water

反応条件

後処理

1. 1
   workup.ADDITIONwas added during the phosgenation
2. 2
   workup.ADDITIONare added as catalyst
3. 3
   その他The aqueous phase is separated off
4. 4
   洗浄washed with distilled water until neutral and free of salt
5. 5
   その他is extruded at 290° C.

実験手順

31 litres of methylene chloride are added to a solution, rendered inert with nitrogen, of 3698.5 g (16.2 mol.) of bisphenol A, 364 g (1.8 mol.) of 4,4′-dihydroxydiphenyl ether and 1584 g (39.6 mol.) of sodium hydroxide in 31 litres of water. In a one-step procedure, 108.14 g (0.72 mol. or 4 mol. % relative to bisphenol A) of p-tert.-butylphenol (BUP) are added as chain terminator. At a pH value of 13.4 and at 21° C., 3560 g (36 mol.) of phosgene are added in the course of 1 hour and 20 minutes. In order to prevent the pH value from falling below 12.6, 25% sodium hydroxide solution was added during the phosgenation. When the phosgenation is complete, and after rinsing with nitrogen, 24.7 ml (0.18 mol., 1 mol. % relative to bisphenol A) of n-ethylpiperidine are added as catalyst, and stirring is then carried out for one hour. The aqueous phase is separated off, and the organic phase is acidified with phosphoric acid and washed with distilled water until neutral and free of salt. After replacing the solvent with chlorobenzene, the product is extruded at 290° C. using an evaporating extruder.

出典