4-hydroxy-2,2,5,5-tetramethylhexan-3-one

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

実験手順: 7.8 g (0.045 moles) of 2,2,5,5-tetramethyl-4-hydroxy-3-hexanone were dissolved in 90 ml of hexane and stirred vigorously with 157 ml of 1M aqueous potassium permanganate solution containing 1.8 g (0.045 moles) of sodium hydroxide. This mixture was then refluxed overnight. The mixture was then cooled to room temperature and the hexane layer separated. The aqueous layer was then extracted three times with 50 ml of hexane. The hexane solutions were then combined and washed three times with 50 ml of pure water before drying over anhydrous magnesium sulfate. The mixture was then filtered and the hexane distilled off at atmospheric pressure to yield 6.3 g of 2,2,5,5-tetramethyl-3,4-hexanedione (82% of theoretical). This mixture was then refluxed overnight the hexane layer separated The aqueous layer was then extracted three times with 50 ml of hexane washed three times with 50 ml of pure water before drying over anhydrous magnesium sulfate The mixture was then filtered the hexane distilled off at atmospheric pressure

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

実験手順: 7.8 g (0.045 moles) of 2,2,5,5-tetramethyl-4-hydroxy-3-hexanone were dissolved in 90 ml of hexane and stirred vigorously with 157 ml of 1M aqueous potassium permanganate solution containing 1.8 g (0.045 moles) of sodium hydroxide. This mixture was then refluxed overnight. The mixture was then cooled to room temperature and the hexane layer separated. The aqueous layer was then extracted three times with 50 ml of hexane. The hexane solutions were then combined and washed three times with 50 ml of pure water before drying over anhydrous magnesium sulfate. The mixture was then filtered and the hexane distilled off at atmospheric pressure to yield 6.3 g of 2,2,5,5-tetramethyl-3,4-hexanedione (82% of theoretical). This mixture was then refluxed overnight the hexane layer separated The aqueous layer was then extracted three times with 50 ml of hexane washed three times with 50 ml of pure water before drying over anhydrous magnesium sulfate The mixture was then filtered the hexane distilled off at atmospheric pressure

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

実験手順: 7.8 g (0.045 moles) of 2,2,5,5-tetramethyl-4-hydroxy-3-hexanone were dissolved in 90 ml of hexane and stirred vigorously with 157 ml of 1M aqueous potassium permanganate solution containing 1.8 g (0.045 moles) of sodium hydroxide. This mixture was then refluxed overnight. The mixture was then cooled to room temperature and the hexane layer separated. The aqueous layer was then extracted three times with 50 ml of hexane. The hexane solutions were then combined and washed three times with 50 ml of pure water before drying over anhydrous magnesium sulfate. The mixture was then filtered and the hexane distilled off at atmospheric pressure to yield 6.3 g of 2,2,5,5-tetramethyl-3,4-hexanedione (82% of theoretical). This mixture was then refluxed overnight the hexane layer separated The aqueous layer was then extracted three times with 50 ml of hexane washed three times with 50 ml of pure water before drying over anhydrous magnesium sulfate The mixture was then filtered the hexane distilled off at atmospheric pressure

反応条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5 g (0.125 mol) of sodium hydroxide powder was added to 11.6 g (0.05 mol) of 4-Bromo-2,2,5,5-tetramethyl-3-hexanone in 10 g of dry diethylformamide. This reaction mixture was heated to 110° C. for 2 hours, cooled to room temperature and 600 mL of water and 200 mL of hexanes added. The hexane layer was collected and the aqueous layer was washed three times with 50 ml of additional hexanes. The hexanes fractions were then combined, washed three times with 50 ml water, then dried with MgSO4. The product was collected as a crystalline solid after hexanes removal by atmospheric distillation. cooled to room temperature The hexane layer was collected the aqueous layer was washed three times with 50 ml of additional hexanes washed three times with 50 ml water dried with MgSO4 The product was collected as a crystalline solid after hexanes removal by atmospheric distillation