2-(3-甲酰基苯氧基)乙腈

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: In 5 ml of chloroform were dissolved 0.57 g of 3-acetyl-4-hydroxy-2H-1-benzopyran-2-one, 0.45 g of 3-(cyanomethoxy)benzaldehyde and 0.20 g of piperidine, and the solution was heated under refluxing for 1 hour and 30 minutes while water was removed with a Soxhlet's extractor filled with a molecular sieve. After cooling to room temperature, the reaction mixture washed successively with 10% hydrochloric acid and an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated. Precipitated crystals were washed with a mixture of 10 ml of dioxane and 10 ml of chloroform, and washed with 10 ml of t-butyl methyl ether to obtain 0.56 g of 4-hydroxy-3-[3-[3-(cyanomethoxy)phenyl]-1-oxo-2-propenyl]-2H-1-benzopyran-2-one [Compound No. (14d)] as a yellow crystal. the solution was heated was removed with a Soxhlet's extractor filled with a molecular sieve the reaction mixture washed successively with 10% hydrochloric acid an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate concentrated Precipitated crystals were washed with a mixture of 10 ml of dioxane and 10 ml of chloroform washed with 10 ml of t-butyl methyl ether

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: In a mixture of 3000 ml of chloroform and 600 ml of dimethylformamide were dissolved 60.00 g of 3-acetyl-4-hydroxy-2(1H)-quinolinone, 142.20 g of 3-(cyanomethoxy)benzaldehyde and 17.64 g of piperidine, and the solution was heated overnight under reflux while water was removed with a Soxhlet extractor filled with molecular sieves. After cooled to room temperature, precipitated crystals were filtered, and washed with 750 ml of tetrahydrofuran and 900 ml of t-butyl methyl ether to obtain 77.59 g of 4-hydroxy-3-[3-[3-(cyanomethoxy)phenyl]-1-oxo-2-propenyl]-2(1H)-quinolinone [Compound No. (10e)] as a yellow crystal. the solution was heated overnight was removed with a Soxhlet extractor filled with molecular sieves precipitated crystals were filtered washed with 750 ml of tetrahydrofuran and 900 ml of t-butyl methyl ether

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

实验步骤: In 5 ml of chloroform were dissolved 0.57 g of 3-acetyl-4-hydroxy-2H-1-benzopyran-2-one, 0.45 g of 3-(cyanomethoxy)benzaldehyde and 0.20 g of piperidine, and the solution was heated under refluxing for 1 hour and 30 minutes while water was removed with a Soxhlet's extractor filled with a molecular sieve. After cooling to room temperature, the reaction mixture washed successively with 10% hydrochloric acid and an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated. Precipitated crystals were washed with a mixture of 10 ml of dioxane and 10 ml of chloroform, and washed with 10 ml of t-butyl methyl ether to obtain 0.56 g of 4-hydroxy-3-[3-[3-(cyanomethoxy)phenyl]-1-oxo-2-propenyl]-2H-1-benzopyran-2-one [Compound No. (14d)] as a yellow crystal. the solution was heated was removed with a Soxhlet's extractor filled with a molecular sieve the reaction mixture washed successively with 10% hydrochloric acid an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate concentrated Precipitated crystals were washed with a mixture of 10 ml of dioxane and 10 ml of chloroform washed with 10 ml of t-butyl methyl ether

反应条件: temp:0.00; pressure:0.00; stir: