2,2,6,6-四甲基环己酮

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 2.3 g of hydroxylamine hydrochloride and 3.6 g of sodium acetate in 20 ml of water is added at RT to a solution of 3.4 g of 2,2,6,6-tetramethylcyclohexanone in 20 ml of MeOH and the reaction mixture is then refluxed for 48 hours. After cooling to RT, the precipitate formed is filtered off, washed with water and dried under vacuum to give 1.2 g of the expected product. the reaction mixture is then refluxed for 48 hours the precipitate formed is filtered off washed with water dried under vacuum

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Magnesium (11.5 g, 0.48 moles) and dried diethyl ether (300 ml) were added, in this order, to one liter four-necked flask equipped with a mechanical stirrer, a dropping funnel, a thermometer, a reflux condenser and a nitrogen gas inlet tube and stirred at room temperature. While stirring at room temperature, a mixed solution of allyl bromide (57.7 g, 0.48 moles)/dried diethyl ether (100 ml) was dropped to the mixture in 2 hours. The resulting mixture was heated under reflux for 30 minutes. Into the mixture was dropped a mixed solution of 2,2,6,6-tetramethylcyclohexanone (49 g, 0.32 moles)/dried diethyl ether (100 ml) in about 40 minutes while stirring under heating and refluxing conditions. The mixture was further stirred for 2 hours under refluxing conditions. The resultant reaction mixture was poured into iced water, followed by adding a 1N hydrochloric acid aqueous solution to render the mixture weakly acidic and separating it into two layers. The organic layer was washed with a saturated sodium bicarbonate aqueous solution (50 ml) and then with water (50 ml) three times. The organic layer was dried over anhydrous magnesium sulfate and separated by filtration, followed by concentration and fractionation to obtain 42.7 g (yield 68%) of the captioned compound. This compound was a colorless transparent liquid having a woody, green, earthy and patchuli oil-like odor. equipped with a mechanical stirrer, a dropping funnel While stirring at room temperature The resulting mixture was heated under reflux for 30 minutes while stirring under heating refluxing conditions The mixture was further stirred for 2 hours under refluxing conditions The resultant reaction mixture separating it into two layers The organic layer was washed with a saturated sodium bicarbonate aqueous solution (50 ml) The organic layer was dried over anhydrous magnesium sulfate separated by filtration followed by concentration and fractionation

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 2.3 g of hydroxylamine hydrochloride and 3.6 g of sodium acetate in 20 ml of water is added at RT to a solution of 3.4 g of 2,2,6,6-tetramethylcyclohexanone in 20 ml of MeOH and the reaction mixture is then refluxed for 48 hours. After cooling to RT, the precipitate formed is filtered off, washed with water and dried under vacuum to give 1.2 g of the expected product. the reaction mixture is then refluxed for 48 hours the precipitate formed is filtered off washed with water dried under vacuum