2-hydroperoxy-2,4,4-trimethylpentane

反応条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 49 g (0.50 mole) of mesityl oxide and 10 g of Amberlyst 15® sulfonic acid type ion-exchange resin was stirred at 0°-5° C., while 78 g (0.45 mole) of 84% 1,1,3,3-tetramethylbutyl hydroperoxide was added slowly. The reaction mixture was allowed to warm to 25° C. and the stirring continued for 16 hours. The ion-exchange resin was separated by filtration. Iodometric assay showed that substantially all of the hydroperoxide had reacted. The infrared spectrum and G.L.C. showed the presence of the desired product. was added slowly The ion-exchange resin was separated by filtration had reacted

反応条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 49 g (0.50 mole) of mesityl oxide and 10 g of Amberlyst 15® sulfonic acid type ion-exchange resin was stirred at 0°-5° C., while 78 g (0.45 mole) of 84% 1,1,3,3-tetramethylbutyl hydroperoxide was added slowly. The reaction mixture was allowed to warm to 25° C. and the stirring continued for 16 hours. The ion-exchange resin was separated by filtration. Iodometric assay showed that substantially all of the hydroperoxide had reacted. The infrared spectrum and G.L.C. showed the presence of the desired product. was added slowly The ion-exchange resin was separated by filtration had reacted

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

実験手順: t-butyl hydroperoxide; cumene hydroperoxide;

反応条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Into the 200 ml jacketed reactor described in Example II were added 18.0 grams (0.152 m) alpha-methylstyrene, 18.4 grams (0.11 m) 87.6% 1,1,3,3-tetramethylbutyl hydroperoxide and 4.6 grams (0.048 m) phenol. The mixture was stirred to obtain a clear solution and the temperature was adjusted to 20° C. To this solution was added 1.7 grams (0.011 m) of t-cumyl chloride from the addition funnel over 5 minutes while holding the temperature at 20°-21° C. The reaction was stirred 5 minutes at 21°-22° C., warmed to 25° C. and stirred 1/2 hour at 25° C., 1/2 hour at 30° C., 1/2 hour at 35° C., 11/2 hours at 40° C. and finally 1/2 hour at 45° C. At this point the t-octyl hydroperoxide had been completely consumed and the reaction was terminated by adding 50 mls of water, stirring 5 minutes, adding 10 mls of 50% NaOH, stirring another 5 minutes and separating the aqueous caustic layer. The organic layer was successively washed with 50 mls 15% NaOH, saturated NaHCO3 solution, H2O, 15% NaHSO3 solution, saturated NaHCO3 solution and water. After drying over anhydrous sodium sulfate the crude product weighed 32.6 grams and contained 72.6% cumyl t-octyl peroxide for a corrected yield of 23.7 grams and a 81.5% yield. to obtain a clear solution was adjusted to 20° C at 20°-21° C The reaction was stirred 5 minutes at 21°-22° C. stirred 1/2 hour at 25° C., 1/2 hour at 30° C., 1/2 hour at 35° C. 2 hours at 40° C. finally 1/2 hour at 45° C At this point the t-octyl hydroperoxide had been completely consumed the reaction was terminated by adding 50 mls of water stirring 5 minutes adding 10 mls of 50% NaOH stirring another 5 minutes separating the aqueous caustic layer The organic layer was successively washed with 50 mls 15% NaOH, saturated NaHCO3 solution, H2O, 15% NaHSO3 solution, saturated NaHCO3 solution and water After drying over anhydrous sodium sulfate the crude product

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a jacketed reactor was charged 8.36g. (0.116 mole) of 2-butanone, 38.0g. (0.232 mole) of 1,1,3,3-tetramethylbutyl hydroperoxide (89.7% assay) and 100 ml. of pentane. To the vigorously stirred mixture at 0°C was added 17.2g. of 77% sulfuric acid over a period of 15 minutes and the mixture was allowed to stir at 0°C for 4 hours. The product was worked up as in Example I and 23.8g. (59.5% of theory, uncorr.) of liquid was obtained which had an active oxygen content of 8.41% (theory, 9.25%). Hence, the assay of the product was 91.0% and the corrected yield was 54.2%. An infrared spectrum of the product showed no OH or C=O bands but showed a strong and broad OO band centered at 875 cm-1. To a jacketed reactor was charged 8.36g To the vigorously stirred mixture at 0°C was added 17.2g (59.5% of theory, uncorr.) of liquid was obtained which

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a jacketed reactor was charged 7.0g. (0.12 mole) of acetone, 39.2g. (0.24 mole) of 1,1,3,3-tetramethylbutyl hydroperoxide (89.7% assay) and 120 ml. of pentane. To the vigorously stirred solution at 0°C was added 16g. of 77% sulfuric acid over a period of 30 minutes and the reaction mixture was allowed to stir at 0°C for 4 hours. The pentane layer was then separated, washed with water, then aqueous 10% KOH solution and finally with water to neutral and was dried over anhyd. MgSO4. After separation of the desiccant and vacuum stripping, 21.3g. (53.1% of theory, uncorr.) of liquid remained which had an "active oxygen" content of 8.66% (theory, 9.64%). Hence, the assay was 90% and the corrected yield was 47.8%. An infrared spectrum of the product showed no O--H or C=O bands but showed a strong OO band at 860 cm-1. To a jacketed reactor was charged 7.0g The pentane layer was then separated washed with water aqueous 10% KOH solution and finally with water to neutral and was dried over anhyd After separation of the desiccant and vacuum stripping, 21.3g

反応条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 49 g (0.50 mole) of mesityl oxide and 10 g of Amberlyst 15® sulfonic acid type ion-exchange resin was stirred at 0°-5° C., while 78 g (0.45 mole) of 84% 1,1,3,3-tetramethylbutyl hydroperoxide was added slowly. The reaction mixture was allowed to warm to 25° C. and the stirring continued for 16 hours. The ion-exchange resin was separated by filtration. Iodometric assay showed that substantially all of the hydroperoxide had reacted. The infrared spectrum and G.L.C. showed the presence of the desired product. was added slowly The ion-exchange resin was separated by filtration had reacted

反応条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 49 g (0.50 mole) of mesityl oxide and 10 g of Amberlyst 15® sulfonic acid type ion-exchange resin was stirred at 0°-5° C., while 78 g (0.45 mole) of 84% 1,1,3,3-tetramethylbutyl hydroperoxide was added slowly. The reaction mixture was allowed to warm to 25° C. and the stirring continued for 16 hours. The ion-exchange resin was separated by filtration. Iodometric assay showed that substantially all of the hydroperoxide had reacted. The infrared spectrum and G.L.C. showed the presence of the desired product. was added slowly The ion-exchange resin was separated by filtration had reacted