phenacyl thiocyanate

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: In a 100 mL three-neck flask, 10.0 g (56.4 mmol) of 2-oxo-2-phenylethyl thiocyanate and 3.73 g (56.4 mmol) of malononitrile were dissolved in 60 mL of ethanol and admixed with 5.14. g (50.8 mmol) of triethylamine in a gradual manner, so the temperature did not climb above 30° C. This was followed by stirring at room temperature for 12 h. The reaction mixture was diluted with 50 mL of water and acidified with glacial acetic acid. The precipitated solid was separated off and washed three times with 10 mL of a 10:10:1 mixture of water:ethanol:glacial acetic acid each time. The solid was dried to obtain 11.1 g (49.1 mmol) of (4-phenyl-1,3-thiazol-2-yl)malononitrile. did not climb above 30° C The precipitated solid was separated off washed three times with 10 mL of a 10:10:1 mixture of water The solid was dried

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

実験手順: 90 parts of phenacyl thiocyanate are introduced into a mixture of 150 parts of DMF, 150 parts of triethylamine and 50 parts of methyl cyanoacetate. The mixture is then stirred for 4 hours at room temperature, after which it is introduced into water and the batch is acidified with acetic acid. The product which precipitates is filtered off and dried in an oven. The product which precipitates is filtered off dried in an oven

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

実験手順: 132 parts of phenacyl thiocyanate, 38 parts of zinc chloride and 129 parts of 1-aminobenzene-3-sulfonic acid are together stirred with 750 parts of water for 20 hours at the boil. After the mixture has cooled, the product is filtered off and dried. After the mixture has cooled the product is filtered off dried

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

実験手順: Following the known process [Bull. Soc. Chem. France, 11, 2498 (1963)], 8.85 g (50 mmol) of α-thiocyanoacetophenone, 5 ml, of water and 1.3 ml of concentrated sulfuric acid were added to 40 ml of acetic acid and the resultant mixture was refluxed for 2 hours. The reaction mixture was then allowed to stand overnight at room temperature. Precipitated crystals were collected by filtration and then washed with water, whereby the title compound was obtained a colorless crystals. Precipitated crystals were collected by filtration washed with water, whereby the title compound was obtained a colorless crystals

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

実験手順: In accordance with the known process (Beilstein, 8, 94), 10.0 g (50 mmol) of o-bromoacetophenone and 4.9 g (50 mmol) of potassium thiocyanate were added to 80 ml of ethyl alcohol, and the resultant mixture was heated at 80° C. for 3 hours and then allowed to stand overnight. Added to the reaction mixture were 50 ml of water. Precipitated crystals were collected by filtration, washed with 50% aqueous ethyl alcohol and then dried, whereby the title compound was obtained as colorless crystals. Added to the reaction mixture Precipitated crystals were collected by filtration washed with 50% aqueous ethyl alcohol dried

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

実験手順: A mixed solution of 2-oxo-2-phenylethyl thiocyanate (5.67 g, 32.0 mmol), water (3.2 ml), concentrated sulfuric acid (0.832 ml) and acetic acid (26 ml) was stirred at 130° C. for 2 hours and at room temperature for 2 hours. A formed precipitate was collected by filtration and washed with water to give 4.78 g (84.3%) of the desired product. A formed precipitate was collected by filtration washed with water

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

実験手順: A mixed solution of 2-oxo-2-phenylethyl thiocyanate (5.67 g, 32.0 mmol), water (3.2 ml), concentrated sulfuric acid (0.832 ml) and acetic acid (26 ml) was stirred at 130° C. for 2 hours and at room temperature for 2 hours. A formed precipitate was collected by filtration and washed with water to give 4.78 g (84.3%) of the desired product. A formed precipitate was collected by filtration washed with water

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

実験手順: A solution of α-bromoacetophenone (10.0 g, 50.0 mmol) and potassium thiocyanate (4.90 g, 50.0 mmol) in ethanol (80 ml) was stirred at 80° C. for 3 hours. After cooling to room temperature, a precipitated solid was collected by filtration, washed with 50% ethanol in water and dried to give 5.99 g (67.6%) of the desired product. a precipitated solid was collected by filtration washed with 50% ethanol in water dried

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

実験手順: A solution of α-bromoacetophenone (10.0 g, 50.0 mmol) and potassium thiocyanate (4.90 g, 50.0 mmol) in ethanol (80 ml) was stirred at 80° C. for 3 hours. After cooling to room temperature, a precipitated solid was collected by filtration, washed with 50% ethanol in water and dried to give 5.99 g (67.6%) of the desired product. a precipitated solid was collected by filtration washed with 50% ethanol in water dried

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

実験手順: To a solution of 1-phenyl-2-thiocyanato-ethanone (20 g, 113 mmol) in HOAc (100 mL) was added 50% aqueous H2SO4 (20 mL). The mixture was refluxed for 10 min. The mixture was poured into water. The solid formed was collected by filtration to give crude 4-phenyl-3H-thiazol-2-one (20 g) which was used for the next step without further purification. The mixture was refluxed for 10 min The solid formed was collected by filtration