Isopropanol → 2-Hydroxyethyl Methacrylate

Participants

Reaction Conditions

Reaction Steps

10.02 g of the intermediate siloxane of formula 5, 15.52 g of ally alcohol (Wako Pure Chemical Industries), 25.04 g of 2-propanol (super dehydrated) (Wako Pure Chemical Industries), 0.20 g of 10% potassium acetate in ethanol, 0.10 g of 1% BHT/IPA, and 0.05 g of 1% MQ/IPA were added into 300 ml eggplant-shaped flask. To this solution 0.40 g of 1% H2PtCl6/6H20/IPA was added and stirred at 50° C. for 13.5 h. After that 0.4128 g of 1% NaHCO3 aq. was added and stirred for over 1 h at room temperature. Then the reaction mixture was evaporated and vacuum dried at 35° C. To this mixture about 5 g of acetone and 15 g of DI water were added with vigorous shaking. The mixture was then centrifuged (7000 rpm, 5° C., 10 min). The upper (aqueous) layer was removed. This operation was repeated three times in total. To this mixture 5 g IPA was added and the reaction mixture was evaporated and vacuum-dried at 40° C. Then 0.06 g of 1% BHT/IPA and 0.03 g of 1% MQ/IPA were added and then evaporated and vacuum-dried at 45° C. The reaction yielded 16.6762 g of a polysiloxane, designated H30AA-5K, having the structure of Formula 3 (above) wherein R2 is a methyl group, m is 0, n is ˜30, and p is 0. The siloxane had an HLB value of about 3 and a hydroxyl content of about 13 wt. %.

Provenance & Evidence