Phosgene → HCID 178439294, compound

Participants

Reaction Steps

A 500 mL Morton flask was charged with BPA (22.8 g, 100 mmol), eugenol siloxane bisphenol (p=19) (3.2 g, 1.8 mmol), p-cumylphenol (0.85 g, 4.0 mmol, 4.0 mol %), methylene chloride (125 mL), distilled water (90 mL) and triethylamine (125 uL, 1 mol %). The pH was adjusted to 10.5 with 50 wt % NaOH. Phosgene (13.2 g, 132 mmol, 30 mol % excess) was added at 0.6 g/min maintaining the pH at 10.5 by the addition of the NaOH solution. Methylene chloride (25 mL) was added. The polymer solution was separated from the brine and washed once with 1N HCl and four times with distilled water. The polymer solution was precipitated into boiling water (750 mL) in a blender, washed with water (500 mL) and dried overnight at 110° C. under vacuum. The product polymer, analyzed by 1H-NMR, showed complete incorporation of the eugenol siloxane bisphenol (9.9 wt %). The product copolycarbonate had a Tg of 140° C. and a weight average molecular weight, Mw, of 57,600. The product copolycarbonate was shown by 1H-NMR to have a blocky structure.

Provenance & Evidence