phenacyl acetate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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: 78.5 g (0.80 mol) of potassium acetate, 5.0 g (0.08 mol) of acetic acid, and 123.7 g (0.80 mol) of 2-chloroacetophenone were heated under reflux in 500 mL of ethanol for 6 hours. After completion of heating, the reaction mixture was cooled to room temperature, deposited potassium chloride was filtered off, and the ethanol was distilled off in vacuo to obtain a pale brown oily material. This oily material was poured into one litter of water, and a precipitated solid was collected by filtration and recrystallized from methanol to obtain 113.1 g (yield: 79.3%) of 2-acetoxyacetophenone as a pale yellow solid. After completion of heating was filtered off the ethanol was distilled off in vacuo to obtain a pale brown oily material a precipitated solid was collected by filtration recrystallized from methanol

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

実験手順: A solution of 2-acetoxyacetophenone (from Example 1) (8.9 g, 0.05M) and α-(benzothiazol-2-yl)-acetate (from Example 3) dissolved in methanol (40 mL) by stirring at room temperature was treated at room temperature with a solution prepared by dissolving sodium hydroxide pellets (2.5 g) in methanol (30 mL) by stirring. A slight exothermic reaction was observed. After being stirred at about room temperature for about 1.0 hour, the reaction mixture was acidified to a pH of about 4 by the dropwise addition of concentrated HCl. The product which was a dark brown colored semi-crystalline mass was washed by decantation and dried in air (yield--12.0 g (81.9% of the theoretical yield). Mass spectrometry indicated that the product largely consisted of the following desired compound: ##STR16## was treated at room temperature with a solution prepared by stirring A slight exothermic reaction After being stirred at about room temperature for about 1.0 hour was washed by decantation dried in air ( yield--12.0 g (81.9% of the theoretical yield)

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2-bromoacetophenone (199 g, 1.0M), acetic acid (200 mL) and acetic anhydride (30 mL) was stirred and heated to about 60° C. Anhydrous sodium acetate (100 g, 1.2M) was added and the reaction mixture was heated and stirred at about 130° C. for 6.0 hrs and then allowed to cool. To remove most of the salt, the reaction mixture was filtered through a sintered glass funnel. The acetic acid and acetic anhydride were removed from the filtrate using a rotary evaporator. A white solid was obtained upon cooling (yield--97.0 g). Mass spectroscopy supported the proposed structure. the reaction mixture was heated stirred at about 130° C. for 6.0 hrs to cool To remove most of the salt the reaction mixture was filtered through a sintered glass funnel The acetic acid and acetic anhydride were removed from the filtrate a rotary evaporator A white solid was obtained upon cooling (yield--97.0 g)

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

実験手順: Five grams of acetic acid are added to 25 mls. of water in a suitable vessel and carefully neutralized with 10% aqueous sodium hydroxide. A few drops of acetic acid are then added until the solution is just acid to litmus paper. Fifty milliliters of ethanol and 5 grams of phenacyl bromide are then added and the mixture is refluxed for 1 hour. If a solid separates during refluxing additional ethanol is added to dissolve the same. The solution is allowed to cool and the phenacyl acetate is recovered by filtration and purified by recrystallization from ethanol, m.p. 47°-48° C. the mixture is refluxed for 1 hour is added to dissolve the same to cool the phenacyl acetate is recovered by filtration purified by recrystallization from ethanol, m.p. 47°-48° C.

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

実験手順: 78.5 g (0.80 mol) of potassium acetate, 5.0 g (0.08 mol) of acetic acid, and 123.7 g (0.80 mol) of 2-chloroacetophenone were heated under reflux in 500 mL of ethanol for 6 hours. After completion of heating, the reaction mixture was cooled to room temperature, deposited potassium chloride was filtered off, and the ethanol was distilled off in vacuo to obtain a pale brown oily material. This oily material was poured into one litter of water, and a precipitated solid was collected by filtration and recrystallized from methanol to obtain 113.1 g (yield: 79.3%) of 2-acetoxyacetophenone as a pale yellow solid. After completion of heating was filtered off the ethanol was distilled off in vacuo to obtain a pale brown oily material a precipitated solid was collected by filtration recrystallized from methanol

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

実験手順: A solution of 2-acetoxyacetophenone (from Example 1) (8.9 g, 0.05M) and α-(benzothiazol-2-yl)-acetate (from Example 3) dissolved in methanol (40 mL) by stirring at room temperature was treated at room temperature with a solution prepared by dissolving sodium hydroxide pellets (2.5 g) in methanol (30 mL) by stirring. A slight exothermic reaction was observed. After being stirred at about room temperature for about 1.0 hour, the reaction mixture was acidified to a pH of about 4 by the dropwise addition of concentrated HCl. The product which was a dark brown colored semi-crystalline mass was washed by decantation and dried in air (yield--12.0 g (81.9% of the theoretical yield). Mass spectrometry indicated that the product largely consisted of the following desired compound: ##STR16## was treated at room temperature with a solution prepared by stirring A slight exothermic reaction After being stirred at about room temperature for about 1.0 hour was washed by decantation dried in air ( yield--12.0 g (81.9% of the theoretical yield)

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

実験手順: A solution of 2-acetoxyacetophenone (from Example 1) (8.9 g, 0.05M) and α-(benzothiazol-2-yl)-acetate (from Example 3) dissolved in methanol (40 mL) by stirring at room temperature was treated at room temperature with a solution prepared by dissolving sodium hydroxide pellets (2.5 g) in methanol (30 mL) by stirring. A slight exothermic reaction was observed. After being stirred at about room temperature for about 1.0 hour, the reaction mixture was acidified to a pH of about 4 by the dropwise addition of concentrated HCl. The product which was a dark brown colored semi-crystalline mass was washed by decantation and dried in air (yield--12.0 g (81.9% of the theoretical yield). Mass spectrometry indicated that the product largely consisted of the following desired compound: ##STR16## was treated at room temperature with a solution prepared by stirring A slight exothermic reaction After being stirred at about room temperature for about 1.0 hour was washed by decantation dried in air ( yield--12.0 g (81.9% of the theoretical yield)

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2-bromoacetophenone (199 g, 1.0M), acetic acid (200 mL) and acetic anhydride (30 mL) was stirred and heated to about 60° C. Anhydrous sodium acetate (100 g, 1.2M) was added and the reaction mixture was heated and stirred at about 130° C. for 6.0 hrs and then allowed to cool. To remove most of the salt, the reaction mixture was filtered through a sintered glass funnel. The acetic acid and acetic anhydride were removed from the filtrate using a rotary evaporator. A white solid was obtained upon cooling (yield--97.0 g). Mass spectroscopy supported the proposed structure. the reaction mixture was heated stirred at about 130° C. for 6.0 hrs to cool To remove most of the salt the reaction mixture was filtered through a sintered glass funnel The acetic acid and acetic anhydride were removed from the filtrate a rotary evaporator A white solid was obtained upon cooling (yield--97.0 g)