Originator
Valbil,Rohm Pharma,W. Germany,1981
Manufacturing Process
Initially, 4.5 g (0.08 mol) pulverized potassium hydroxide was dissolved in
300 ml isopropanol in a 500 ml four-neck flask equipped with stirrer, intensive
cooler, dropping funnel and feed pipe for the gas treatment with nitrogen.
Then, 52.0 g (0.4 mol) n-butylglycidyl ether and 41.4 g (0.44 mol) phenol
was added thereto, whereafter the material was heated to boiling under
nitrogen. The material was stirred, about 8.5 hours, until no glycidyl ether
could be determined, e.g., by gas chromatography.
After the suspension was cooled under nitrogen, the solvent was distilled off
under vacuum. The residue was taken up in 200 ml water and the milky
emulsion extracted exhaustively with ether. From the organic phase, the
excess butylglycidyl ether was extracted with diluted potassium hydroxide
solution. The ether phase was washed neutral with water and the solvent
removed after drying with sodium sulfate. The remaining oily residue was
distilled under vacuum; there was obtained a colorless liquid of BP
123.5°C/0.07 mm. Yield: 81.8 g (91.1% of the theory)