methyl 5-chloro-2,4-dihydroxybenzoate

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: A mixture of 1-(chloromethyl)-4-methoxybenzene (1.53 g, 9.8 mmol), methyl 5-chloro-2,4-dihydroxybenzoate (1.98 g, 9.8 mmol) and potassiumcarbonate (1.35 g, 9.8 mmol) in acetone (15 mL) was stirred at reflux overnight. The mixture was filtered, solvent was removed in vacuo, the residue was dissolved in ethyl acetate and was washed with brine two times. The organic layer was dried over sodium sulphate, solvent was removed in vacuo and the residue was purified by recrystillaziation from methanol. (1.46 g, 46%) of the title compound was obtained. at reflux overnight The mixture was filtered solvent was removed in vacuo the residue was dissolved in ethyl acetate was washed with brine two times The organic layer was dried over sodium sulphate, solvent was removed in vacuo the residue was purified by recrystillaziation from methanol

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

実験手順: A mixture of 1-(chloromethyl)-4-methoxybenzene (1.53 g, 9.8 mmol), methyl 5-chloro-2,4-dihydroxybenzoate (1.98 g, 9.8 mmol) and potassiumcarbonate (1.35 g, 9.8 mmol) in acetone (15 mL) was stirred at reflux overnight. The mixture was filtered, solvent was removed in vacuo, the residue was dissolved in ethyl acetate and was washed with brine two times. The organic layer was dried over sodium sulphate, solvent was removed in vacuo and the residue was purified by recrystillaziation from methanol. (1.46 g, 46%) of the title compound was obtained. at reflux overnight The mixture was filtered solvent was removed in vacuo the residue was dissolved in ethyl acetate was washed with brine two times The organic layer was dried over sodium sulphate, solvent was removed in vacuo the residue was purified by recrystillaziation from methanol

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

実験手順: To a solution of methyl 5-chloro-2,4-dihydroxybenzoate (0.41 g, 2 mmol) in acetone were added 1-(chloromethyl)-4-methoxybenzene (0.32 g, 2 mmol) and K2CO3 (0.28 g, 2 mmol). The reaction mixture was heated with reflux for 3 days, than cooled to room temperature. The inorganic material was removed by filtration. The solvent was distilled in vacuo, and the residue was recrystallized from methanol to afford white solid (0.37 g, 60%). The reaction mixture was heated with reflux for 3 days The inorganic material was removed by filtration The solvent was distilled in vacuo the residue was recrystallized from methanol

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

実験手順: To a solution of methyl 5-chloro-2,4-dihydroxybenzoate (0.41 g, 2 mmol) in acetone were added 1-(chloromethyl)-4-methoxybenzene (0.32 g, 2 mmol) and K2CO3 (0.28 g, 2 mmol). The reaction mixture was heated with reflux for 3 days, than cooled to room temperature. The inorganic material was removed by filtration. The solvent was distilled in vacuo, and the residue was recrystallized from methanol to afford white solid (0.37 g, 60%). The reaction mixture was heated with reflux for 3 days The inorganic material was removed by filtration The solvent was distilled in vacuo the residue was recrystallized from methanol

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

実験手順: A mixture of 1-(chloromethyl)-4-methoxybenzene (1.53 g, 9.8 mmol), methyl 5-chloro-2,4-dihydroxybenzoate (1.98 g, 9.8 mmol) and potassiumcarbonate (1.35 g, 9.8 mmol) in acetone (15 mL) was stirred at reflux overnight. The mixture was filtered, solvent was removed in vacuo, the residue was dissolved in ethyl acetate and was washed with brine two times. The organic layer was dried over sodium sulphate, solvent was removed in vacuo and the residue was purified by recrystillaziation from methanol. (1.46 g, 46%) of the title compound was obtained. at reflux overnight The mixture was filtered solvent was removed in vacuo the residue was dissolved in ethyl acetate was washed with brine two times The organic layer was dried over sodium sulphate, solvent was removed in vacuo the residue was purified by recrystillaziation from methanol

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

実験手順: To a solution of methyl 5-chloro-2,4-dihydroxybenzoate (0.41 g, 2 mmol) in acetone were added 1-(chloromethyl)-4-methoxybenzene (0.32 g, 2 mmol) and K2CO3 (0.28 g, 2 mmol). The reaction mixture was heated with reflux for 3 days, than cooled to room temperature. The inorganic material was removed by filtration. The solvent was distilled in vacuo, and the residue was recrystallized from methanol to afford white solid (0.37 g, 60%). The reaction mixture was heated with reflux for 3 days The inorganic material was removed by filtration The solvent was distilled in vacuo the residue was recrystallized from methanol

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

実験手順: To a solution of methyl 5-chloro-2,4-dihydroxybenzoate (0.41 g, 2 mmol) in acetone were added 1-(chloromethyl)-4-methoxybenzene (0.32 g, 2 mmol) and K2CO3 (0.28 g, 2 mmol). The reaction mixture was heated with reflux for 3 days, than cooled to room temperature. The inorganic material was removed by filtration. The solvent was distilled in vacuo, and the residue was recrystallized from methanol to afford white solid (0.37 g, 60%). The reaction mixture was heated with reflux for 3 days The inorganic material was removed by filtration The solvent was distilled in vacuo the residue was recrystallized from methanol

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: To a solution of methyl 5-chloro-2,4-dihydroxybenzoate (0.41 g, 2 mmol) in acetone were added 1-(chloromethyl)-4-methoxybenzene (0.32 g, 2 mmol) and K2CO3 (0.28 g, 2 mmol). The reaction mixture was heated with reflux for 3 days, than cooled to room temperature. The inorganic material was removed by filtration. The solvent was distilled in vacuo, and the residue was recrystallized from methanol to afford white solid (0.37 g, 60%). The reaction mixture was heated with reflux for 3 days The inorganic material was removed by filtration The solvent was distilled in vacuo the residue was recrystallized from methanol

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

実験手順: A mixture of 1-(chloromethyl)-4-methoxybenzene (1.53 g, 9.8 mmol), methyl 5-chloro-2,4-dihydroxybenzoate (1.98 g, 9.8 mmol) and potassiumcarbonate (1.35 g, 9.8 mmol) in acetone (15 mL) was stirred at reflux overnight. The mixture was filtered, solvent was removed in vacuo, the residue was dissolved in ethyl acetate and was washed with brine two times. The organic layer was dried over sodium sulphate, solvent was removed in vacuo and the residue was purified by recrystillaziation from methanol. (1.46 g, 46%) of the title compound was obtained. at reflux overnight The mixture was filtered solvent was removed in vacuo the residue was dissolved in ethyl acetate was washed with brine two times The organic layer was dried over sodium sulphate, solvent was removed in vacuo the residue was purified by recrystillaziation from methanol

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

実験手順: To a solution of methyl 5-chloro-2,4-dihydroxybenzoate (0.41 g, 2 mmol) in acetone were added 1-(chloromethyl)-4-methoxybenzene (0.32 g, 2 mmol) and K2CO3 (0.28 g, 2 mmol). The reaction mixture was heated with reflux for 3 days, than cooled to room temperature. The inorganic material was removed by filtration. The solvent was distilled in vacuo, and the residue was recrystallized from methanol to afford white solid (0.37 g, 60%). The reaction mixture was heated with reflux for 3 days The inorganic material was removed by filtration The solvent was distilled in vacuo the residue was recrystallized from methanol