反应详情

A jacketed reactor equipped with a mechanical stirrer, a thermometer and a dropping funnel was charged with 19.9 g (0.160 mole) of 45% KOH, 9.9 g of water, 21.5 g (0.150 mole) of 93.7% 3-hydroxy-1,1-dimethyl butyl hydroperoxide (also known as 4-hydroxy-2-methyl-2-hydroperoxypentane), 25 g of methylene chloride and 0.65 g (0.002 mole) of tetrabutylammonium bromide, a phase transfer catalyst (PTC). The resulting vigorously stirred mixture was cooled to -5° to -2° C. and to it was slowly added 12.6 g (0.100 mole) of 95.4% pivaloyl chloride over a period of about 30 minutes. The resulting product mixture was then stirred for 2 hours at -5° to -2° C. after which 25 g of 10% KOH and an additional 50 g of methylene chloride were added to the reaction mixture. The reaction mass was allowed to separate into two liquid phases at 10° C. and the lower organic layer was removed, dried over about 5% by weight of anhydrous MgSO4 and after the spent desiccant was separated by filtration the methylene chloride was removed in vacuo at 0° to 10° C. Obtained was 24.5 g of liquid product which had an assay of 72.3% according to peroxyester active oxygen content. The corrected yield was 81.3%. An infrared spectrum of the product showed a large broad OH band centered at 3450 to 3550 cm-1.

1. customA jacketed reactor equipped with a mechanical stirrer
2. temperatureThe resulting vigorously stirred mixture was cooled to -5° to -2° C. and to it
3. customof about 30 minutes
4. customto separate into two liquid phases at 10° C.
5. customthe lower organic layer was removed
6. dry with materialdried over about 5% by weight of anhydrous MgSO4
7. customafter the spent desiccant was separated by filtration the methylene chloride
8. customwas removed in vacuo at 0° to 10° C
9. customObtained