7,7-dimethyloctanoyl chloride

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: Reacting neodecanoyl chloride with 2,5-dimethyl-2,5-dihydroperoxyhexane followed by reducing the intermediate product with a buffered sodium sulfite solution employing the same procedure as used in preparation of C-5 resulted in the preparation of 4-hydroxy-1,1,4,4-tetramethylbutyl peroxyneodecanoate. The liquid product had an assay of 91.7% and was obtained in a corrected yield of 55.1%. An infrared spectrum of the product showed a broad OH band centered at 3300 to 3500 cm-1. as used in preparation of C-5

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

実験手順: Reacting neodecanoyl chloride with 2,5-dimethyl-2,5-dihydroperoxyhexane followed by reducing the intermediate product with a buffered sodium sulfite solution employing the same procedure as used in preparation of C-5 resulted in the preparation of 4-hydroxy-1,1,4,4-tetramethylbutyl peroxyneodecanoate. The liquid product had an assay of 91.7% and was obtained in a corrected yield of 55.1%. An infrared spectrum of the product showed a broad OH band centered at 3300 to 3500 cm-1. as used in preparation of C-5

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: One liter capacity four-necked flask equipped with an agitator is charged with 216.4 g of a 35% KOH aqueous solution, and added under agitation with 289.7 g of 52.9% pinane hydroperoxide, while retaining the solution temperature at 20° C. Further 143.1 g of neodecanoic acid chloride is added dropwise over 10 min., while agitating and retaining the solution temperature at 20° C. After agitation of 1 hr., 170 g of cold water is added to the solution, and additional agitation is effected for 5 min. Then, the solution is left still for phase separation. Water phase is removed by separation to leave an oily phase. The oily phase is washed with 300 g of 5% NaOH aqueous solution, subsequently three times with water, and dried over anhydrous magnesium sulfate. Thus, 325.2 g of pinane peroxyneodecanoate solution of a purity of 54.5% is obtained. Yield is 72.8 mol%. One liter capacity four-necked flask equipped with an agitator at 20° C at 20° C After agitation of 1 hr Then, the solution is left still for phase separation Water phase is removed by separation to leave an oily phase The oily phase is washed with 300 g of 5% NaOH aqueous solution, subsequently three times with water dried over anhydrous magnesium sulfate

反応条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a four-necked flask of 200 ml provided with a stirrer was charged 33.7 g of an aqueous solution of 30% potassium hydroxide, to which was added a mixture of 22.1 g of 95% 1-phenylcyclohexyl hydroperoxide and 30 g of benzene while the liquid temperature was maintained at 10° C. with stirring. Furthermore, 19.1 g of neodecanoyl chloride was added dropwise over 7 minutes while the liquid temperature was maintained at 15° C. with stirring. After the liquid temperature was raised to 25° C. and the stirring was continued for 2 hours, 40 g of cold water was added and further the stirring was made for 5 minutes. The water phase was separated and washed with an aqueous solution of 40 g of 5% sodium hydroxide and further with water three times. The solution was dried on magnesium sulfate anhydride and benzene was removed off under vacuum to obtain 24.0 g of a desired compound as a light yellow liquid. This compound had an active oxygen amount of 4.20%, a purity of 91% through calculation and a yield of 63 mol %. In a four-necked flask of 200 ml provided with a stirrer to which was added was maintained at 15° C. with stirring After the liquid temperature was raised to 25° C. further the stirring was made for 5 minutes The water phase was separated washed with an aqueous solution of 40 g of 5% sodium hydroxide and further with water three times The solution was dried on magnesium sulfate anhydride and benzene was removed off under vacuum

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

実験手順: Reacting neodecanoyl chloride with 2,5-dimethyl-2,5-dihydroperoxyhexane followed by reducing the intermediate product with a buffered sodium sulfite solution employing the same procedure as used in preparation of C-5 resulted in the preparation of 4-hydroxy-1,1,4,4-tetramethylbutyl peroxyneodecanoate. The liquid product had an assay of 91.7% and was obtained in a corrected yield of 55.1%. An infrared spectrum of the product showed a broad OH band centered at 3300 to 3500 cm-1. as used in preparation of C-5

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

実験手順: Reacting neodecanoyl chloride with 2,5-dimethyl-2,5-dihydroperoxyhexane followed by reducing the intermediate product with a buffered sodium sulfite solution employing the same procedure as used in preparation of C-5 resulted in the preparation of 4-hydroxy-1,1,4,4-tetramethylbutyl peroxyneodecanoate. The liquid product had an assay of 91.7% and was obtained in a corrected yield of 55.1%. An infrared spectrum of the product showed a broad OH band centered at 3300 to 3500 cm-1. as used in preparation of C-5