Phosgene → Monoisobutyl phthalate

Participants

Reaction Steps

A solution of MIBP was prepared by dissolving (5.32 g, 0.0168 moles) MIBP monomer (prepared according to Example 7) in 33% aqueous caustic (7 g) and water (30 mL). To a 2 L glass reactor equipped with pH probe, condenser, agitator, phosgene inlet, and caustic scrubber was added methylene chloride (500 mL), deionized water (140 mL), bisphenol-A (4.68 g, 0.0205 moles), triethylamine (0.10 mL, 0.0007 moles), p-cumylphenol (0.24 g, 0.0011 moles), and MIBP solution. The batch was phosgenated in excess at a rate of 2 grams per min for 2 minutes, maintaining the pH between 9 and 10 with concomitant caustic addition (33% w/w). At the completion of the phosgenation, the reactor was purged with nitrogen to remove excess phosgene. The reaction mixture extracted with dilute acid (1N HCl) and deionized water. The final product was isolated as a white powder by exposing the polymer solution (in methylene chloride) to hot water, evaporating the solvent and providing a white powder. Characterization data for the MIBP-BPA Copolymer (PL-11-116) is provided in Table 1, shown below.

Provenance & Evidence