Phosgene → HCID 178439294, compound

Participants

Reaction Steps

A 500 mL Morton flask was charged with BPA (22.8 g, 100 mmol), p-cumylphenol (1.06 g, 5.0 mmol), methylene chloride (125 mL), distilled water (90 mL), triethylamine (125 microliters) and eugenol siloxane bisphenol (3.2 g, 3 mmol) having a value of “p” of about 9. The pH was adjusted to about 10.5 with a solution of 50 percent by weight NaOH in water. Phosgene (13.2 g, 132 mmol) was added at 0.6 g/min while maintaining the pH at about 10.5 by the addition of a solution of 50 percent by weight NaOH in water. Methylene chloride (25 mL) was added and the organic phase was separated from the brine and washed once with 1 N HCl and four times with distilled water. The product polymer was isolated by the addition of the washed methylene chloride solution to boiling water (750 mL) at high shear. The flocculant powder was filtered, washed with distilled water (500 mL) and dried for 24 hr under vacuum at 110° C. The product silicone copolycarbonate had a Tg of 134° C. and a weight average molecular weight (Mw) of 40,700 as determined by gel permeation chromatography (gpc). 1H-NMR in CDCL3 solution revealed the complete incorporation of the eugenol siloxane bisphenol. The product copolycarbonate was further shown by 1H-NMR to have a blocky structure.

Provenance & Evidence