BE810181A - Glycidyl ethers of mono/polyvalent phenols prepn - by reacting phenol with epichlorohydrin and treating prod. with alkali metal hydroxide in two stages - Google Patents

Abstract

Glycidyl ethers are prepd. by reacting corresp. phenol with excess epichlorohydrin in the presence of 0.001-5 esp. 0.01-1 wt. %, w.r.t. phenol, of a divalent Sn cpd. this mixt. being reacted with 0.9-1.15 equivs. of a solid alkali metal hydroxide per phenolic hydroxyl gp. Reaction is effected by (a) forming >=10 esp. 50-90% chlorohydrin ethers w.r.t. phenolic hydroxyl gps. in a medium without alkali, (b) adding 10-90 esp. 15-50 wt. % solid alkali metal hydroxide in 8-90 esp. 15-50% of the total addn. time of solid alkali metal hydroxide, this being 30-300 esp. 90-180 mins., with elimination of the heat of reaction by cooling or distn. under reflux at reduced press. in presence of water of reaction, and opt. of added water, (c) adding 90-10 esp. 85-50 wt. % solid alkali metal hydroxide in 92-10 esp. 85-50% of total addn. time of solid alkali metal hydroxide with elimination of the heat of reaction, the water of reaction, and opt. of the added water by azeotropic distn. and (d) eliminating excess epichlorohydrin from the glycidyl ether by distn. and if the glycidyl ether contains >0.1 wt. % saponifiable Cl, dissolving the ether in an inert solvent and subjecting to dehydrochlorination with the air of excess aq. alkali metal hydroxide soln. w.r.t. hydrolysable Cl. High yields of high quality prods are obtd. economically in short reaction time.