1h nmr and 29si nmr spectroscopy

Example 5

Synthesis of Resin A-5

A 3-L flask equipped with a stirrer, thermometer, nitrogen purge line and reflux condenser was charged with 274.4 g (0.70 mol) of Compound (S-4) and 79.5 g (0.30 mol) of Compound (S-5), then with 2,000 g of toluene and heated at 70° C. Thereafter, 1.0 g of a toluene solution of chloroplatinic acid (platinum concentration 0.5 wt %) was added, and 58.2 g (0.30 mol) of Compound (S-1) and 1109.5 g (0.70 mol) of Compound (S-2) (y¹=20) were added dropwise over 1 hour. The ratio of the total moles of hydrosilyl groups to the total moles of alkenyl groups was 1/1. At the end of dropwise addition, the reaction to solution was heated at 100° C. and aged for 6 hours. Toluene was distilled off in vacuum from the reaction solution, yielding Resin A-5. On analysis by ¹H-NMR and ²⁹Si-NMR spectroscopy (Bruker Corp.) and GPC, the structure of Resin A-5 was identified. Resin A-5 had a Mw of 42,000 and a silicone content of 72.9 wt %.

Example 4

Synthesis of Resin A

A 3-L flask equipped with a stirrer, thermometer, nitrogen purge line and reflux condenser was charged with 325.0 g (0.5 mol) of benzoxazole compound S-1a and 2,000 g of toluene and heated at 70° C. Thereafter, 1.0 g of a toluene solution of chloroplatinic acid (platinum concentration 0.5 wt %) was added, and 755.0 g (0.25 mol) of the compound having formula (S-2) wherein d=40 (Shin-Etsu Chemical Co., Ltd.) and 48.5 g (0.25 mol) of the compound having formula (S-4) (Shin-Etsu Chemical Co., Ltd.) were added dropwise over 1 hour. The molar ratio of the total amount of hydrosilyl groups to the total amount of alkenyl groups was 1/1. At the end of dropwise addition, the reaction solution was heated at 100° C. and aged for 6 hours. Toluene was distilled off in vacuum from the reaction solution, yielding Resin A. On ¹H-NMR and ²⁹Si-NMR spectroscopy (Bruker Corp.), Resin A was identified to comprise repeating units of formulae (1a) and (1b). Resin A had a Mw of 42,000 and a silicone content of 66.9 wt %. In formulae (1a) and (1b), a=0.5 and b=0.5.

Example 6

Synthesis of Resin A-6

A 3-L flask equipped with a stirrer, thermometer, nitrogen purge line and reflux condenser was charged with 55.8 g (0.30 mol) of Compound (S-3), 117.6 g (0.30 mol) of Compound (S-4), and 106.0 g (0.40 mol) of Compound (S-5), then with 2,000 g of toluene and heated at 70° C. Thereafter, 1.0 g of a toluene solution of chloroplatinic acid (platinum concentration 0.5 wt %) was added, and 135.8 g (0.70 mol) of Compound (S-1) and 475.5 g (0.30 mol) of Compound (S-2) (y¹=20) were added dropwise over 1 hour. The ratio of the total moles of hydrosilyl groups to the total moles of alkenyl groups was 1/1. At the end of dropwise addition, the reaction solution was heated at 100° C. and aged for 6 hours. Toluene was distilled off in vacuum from the reaction solution, yielding Resin A-6. On analysis by ¹H-NMR and ²⁹Si-NMR spectroscopy (Bruker Corp.) and GPC, the structure of Resin A-6 was identified. Resin A-6 had a Mw of 31,000 and a silicone content of 59.6 wt %.