N,N,3-triphenylprop-2-enamide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The N,N-diphenylstyrenyl carboxamide-2% divinylbenzene copolymer from example 7(a) (53.0g) was heated with stirring at 130°-135° for 44 hours with a mixture of glacial acetic acid (670 ml.), concentrated sulphuric acid (500 ml.) and water (300 ml.). After cooling to room temperature, the mixture was filtered and the polymer washed successively with water (4 × 400 ml.), acetone (3 × 200 ml.); methanol (3 × 200ml.), water (2 × 400 ml.) and acetone (2 × 200 ml.); and dried in vacuo at 40° to constant weight. The title polymer (36.58g) was green in colour and exhibited ν max (NuJol) 1690 (C=O) and 3700-2400 (OH) cm-1. Titration was effected by suspending the product (0.500g) in 95% ethanol (50 ml.) adding 0.5M sodium hydroxide (50 ml.), warming the mixture to reflux, cooling and back titrating with 0.5M hydrochloric acid using phenolphthalein as the indicator; it was found that 47.12 ml. of acid were required for neutralisation indicating 2.88 m.mole carboxyl/g of polymer. the mixture was filtered the polymer washed successively with water (4 × 400 ml.), acetone (3 × 200 ml.) and dried in vacuo at 40° to constant weight adding 0.5M sodium hydroxide (50 ml.) warming the mixture to reflux cooling

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The N,N-diphenylstyrenyl carboxamide-2% divinylbenzene copolymer from example 7(a) (53.0g) was heated with stirring at 130°-135° for 44 hours with a mixture of glacial acetic acid (670 ml.), concentrated sulphuric acid (500 ml.) and water (300 ml.). After cooling to room temperature, the mixture was filtered and the polymer washed successively with water (4 × 400 ml.), acetone (3 × 200 ml.); methanol (3 × 200ml.), water (2 × 400 ml.) and acetone (2 × 200 ml.); and dried in vacuo at 40° to constant weight. The title polymer (36.58g) was green in colour and exhibited ν max (NuJol) 1690 (C=O) and 3700-2400 (OH) cm-1. Titration was effected by suspending the product (0.500g) in 95% ethanol (50 ml.) adding 0.5M sodium hydroxide (50 ml.), warming the mixture to reflux, cooling and back titrating with 0.5M hydrochloric acid using phenolphthalein as the indicator; it was found that 47.12 ml. of acid were required for neutralisation indicating 2.88 m.mole carboxyl/g of polymer. the mixture was filtered the polymer washed successively with water (4 × 400 ml.), acetone (3 × 200 ml.) and dried in vacuo at 40° to constant weight adding 0.5M sodium hydroxide (50 ml.) warming the mixture to reflux cooling