1-Phenylmethyl-5-phenyl-barbituric acid

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

実験手順: To 64 ml of 50% ethanol, 300 ml (844 mmol) of phosphorus oxychloride was added drop by drop, with stirring under ice cooling conditions. To this solution, 120 g (380 mmol) of 3-benzyl-5-phenylpyrimidine-2,4,6(1H,3H)-trione was added little by little. This mixture was stirred at 50° C. for 30 minutes and then at 100° C. for 90 minutes. After cooling, the reaction mixture was poured into ice water and stirred for 1 hour. The resulting precipitate was collected by filtration, washed with water and n-hexane and dried to yield 112.89 g (94.7%, light white crystal) of the desired product. This mixture was stirred at 50° C. for 30 minutes After cooling stirred for 1 hour The resulting precipitate was collected by filtration washed with water and n-hexane dried

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

実験手順: To a suspension of 100 g (666 mmol) of benzylurea and 156.8 g (666 mmol) of diethyl phenylmalonate in 340 ml of methanol, 164 ml (666 mmol) of a 4.1M sodium methylate solution was added at room temperature, followed by refluxing for 16 hours. After the reaction mixture was cooled, the solvent was distilled off. After the residue was dissolved in water and insoluble substances were filtered out, the filtrate was adjusted to pH 3-4 by adding concentrated hydrochloric acid. The resulting precipitate was collected by filtration, washed with water and n-hexane-diethyl ether and dried to yield 163.23 g (83.3%, white crystal) of the desired product. was added at room temperature by refluxing for 16 hours After the reaction mixture was cooled the solvent was distilled off After the residue was dissolved in water insoluble substances were filtered out by adding concentrated hydrochloric acid The resulting precipitate was collected by filtration washed with water and n-hexane-diethyl ether dried

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

実験手順: To 64 ml of 50% ethanol, 300 ml (844 mmol) of phosphorus oxychloride was added drop by drop, with stirring under ice cooling conditions. To this solution, 120 g (380 mmol) of 3-benzyl-5-phenylpyrimidine-2,4,6(1H,3H)-trione was added little by little. This mixture was stirred at 50° C. for 30 minutes and then at 100° C. for 90 minutes. After cooling, the reaction mixture was poured into ice water and stirred for 1 hour. The resulting precipitate was collected by filtration, washed with water and n-hexane and dried to yield 112.89 g (94.7%, light white crystal) of the desired product. This mixture was stirred at 50° C. for 30 minutes After cooling stirred for 1 hour The resulting precipitate was collected by filtration washed with water and n-hexane dried

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

実験手順: To a suspension of 100 g (666 mmol) of benzylurea and 156.8 g (666 mmol) of diethyl phenylmalonate in 340 ml of methanol, 164 ml (666 mmol) of a 4.1M sodium methylate solution was added at room temperature, followed by refluxing for 16 hours. After the reaction mixture was cooled, the solvent was distilled off. After the residue was dissolved in water and insoluble substances were filtered out, the filtrate was adjusted to pH 3-4 by adding concentrated hydrochloric acid. The resulting precipitate was collected by filtration, washed with water and n-hexane-diethyl ether and dried to yield 163.23 g (83.3%, white crystal) of the desired product. was added at room temperature by refluxing for 16 hours After the reaction mixture was cooled the solvent was distilled off After the residue was dissolved in water insoluble substances were filtered out by adding concentrated hydrochloric acid The resulting precipitate was collected by filtration washed with water and n-hexane-diethyl ether dried

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

実験手順: To a suspension of 100 g (666 mmol) of benzylurea and 156.8 g (666 mmol) of diethyl phenylmalonate in 340 ml of methanol, 164 ml (666 mmol) of a 4.1M sodium methylate solution was added at room temperature, followed by refluxing for 16 hours. After the reaction mixture was cooled, the solvent was distilled off. After the residue was dissolved in water and insoluble substances were filtered out, the filtrate was adjusted to pH 3-4 by adding concentrated hydrochloric acid. The resulting precipitate was collected by filtration, washed with water and n-hexane-diethyl ether and dried to yield 163.23 g (83.3%, white crystal) of the desired product. was added at room temperature by refluxing for 16 hours After the reaction mixture was cooled the solvent was distilled off After the residue was dissolved in water insoluble substances were filtered out by adding concentrated hydrochloric acid The resulting precipitate was collected by filtration washed with water and n-hexane-diethyl ether dried

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

実験手順: Separately, 40 g of distilled water and 6 g of acetone were added to a 200 mL beaker, and 17.29 g of 1-benzyl-5-phenylbarbituric acid (BPBA)(58.74 mmol) was added thereto and the mixture was dispersed homogeneously to obtain an aqueous BPBA/acetone solution. was added the mixture was dispersed homogeneously

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

実験手順: To 64 ml of 50% ethanol, 300 ml (844 mmol) of phosphorus oxychloride was added drop by drop, with stirring under ice cooling conditions. To this solution, 120 g (380 mmol) of 3-benzyl-5-phenylpyrimidine-2,4,6(1H,3H)-trione was added little by little. This mixture was stirred at 50° C. for 30 minutes and then at 100° C. for 90 minutes. After cooling, the reaction mixture was poured into ice water and stirred for 1 hour. The resulting precipitate was collected by filtration, washed with water and n-hexane and dried to yield 112.89 g (94.7%, light white crystal) of the desired product. This mixture was stirred at 50° C. for 30 minutes After cooling stirred for 1 hour The resulting precipitate was collected by filtration washed with water and n-hexane dried

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

実験手順: To a suspension of 100 g (666 mmol) of benzylurea and 156.8 g (666 mmol) of diethyl phenylmalonate in 340 ml of methanol, 164 ml (666 mmol) of a 4.1M sodium methylate solution was added at room temperature, followed by refluxing for 16 hours. After the reaction mixture was cooled, the solvent was distilled off. After the residue was dissolved in water and insoluble substances were filtered out, the filtrate was adjusted to pH 3-4 by adding concentrated hydrochloric acid. The resulting precipitate was collected by filtration, washed with water and n-hexane-diethyl ether and dried to yield 163.23 g (83.3%, white crystal) of the desired product. was added at room temperature by refluxing for 16 hours After the reaction mixture was cooled the solvent was distilled off After the residue was dissolved in water insoluble substances were filtered out by adding concentrated hydrochloric acid The resulting precipitate was collected by filtration washed with water and n-hexane-diethyl ether dried