(2-methoxyphenyl) benzoate

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 stirred solution of 2-methoxyphenyl benzoate (10 g) in dichloromethane (100 mL) from 0°-5° C. is treated dropwise with chlorosulfonic acid (2.9 mL) and the solution is then stirred for 3 hours from 0°-5° C. The precipitate which forms is filtered off, washed with cold dichloromethane, and dried in vacuo, to give 3-benzoyloxy-4-methoxybenzenesulfonic acid (11.45 g), in the form of a white solid, m.p. 139°-140° C. The precipitate which forms is filtered off washed with cold dichloromethane dried in vacuo

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

実験手順: A stirred solution of 2-methoxyphenyl benzoate (10 g) in dichloromethane (100 mL) from 0°-5° C. is treated dropwise with chlorosulfonic acid (2.9 mL) and the solution is then stirred for 3 hours from 0°-5° C. The precipitate which forms is filtered off, washed with cold dichloromethane, and dried in vacuo, to give 3-benzoyloxy-4-methoxybenzenesulfonic acid (11.45 g), in the form of a white solid, m.p. 139°-140° C. The precipitate which forms is filtered off washed with cold dichloromethane dried in vacuo

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

実験手順: A stirred solution of 2-methoxyphenyl benzoate (10 g) in dichloromethane (100 mL) from 0°-5° C. is treated dropwise with chlorosulfonic acid (2.9 mL) and the solution is then stirred for 3 hours from 0°-5° C. The precipitate which forms is filtered off, washed with cold dichloromethane, and dried in vacuo, to give 3-benzoyloxy-4-methoxybenzenesulfonic acid (11.45 g), in the form of a white solid, m.p. 139°-140° C. The precipitate which forms is filtered off washed with cold dichloromethane dried in vacuo

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 stirred solution of 2-methoxyphenyl benzoate (10 g) in dichloromethane (100 mL) from 0°-5° C. is treated dropwise with chlorosulfonic acid (2.9 mL) and the solution is then stirred for 3 hours from 0°-5° C. The precipitate which forms is filtered off, washed with cold dichloromethane, and dried in vacuo, to give 3-benzoyloxy-4-methoxybenzenesulfonic acid (11.45 g), in the form of a white solid, m.p. 139°-140° C. The precipitate which forms is filtered off washed with cold dichloromethane dried in vacuo

反応条件: temp:2.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A stirred solution of 2-methoxyphenyl benzoate (10 g) in dichloromethane (100 mL) from 0-5° C. is treated dropwise with chlorosulfonic acid (2.9 mL) and the solution is then stirred for 3 hours from 0-5° C. The precipitate which forms is filtered off, washed with cold dichloromethane, and dried in vacuo, to give 3-benzoyloxy-4-methoxybenzenesulfonic acid (11.45 g), in the form of a white solid, m.p. 139-140° C. The precipitate which forms is filtered off washed with cold dichloromethane dried in vacuo

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

実験手順: A stirred solution of 2-methoxyphenyl benzoate (29.1 g) in glacial acetic acid (150 mL) is treated with a solution of bromine (7.2 mL) in glacial acetic acid (25 mL) during a period of 20 minutes, and the solution is then stirred for a further period of 30 minutes at room temperature. The mixture is concentrated in vacuo, and the resulting residue is dissolved in methyl t-butyl ether (200 mL), washed with water (100 mL) and saturated aqueous sodium bicarbonate solution (3×100 mL), dried over magnesium sulphate and evaporated. The resulting residue is recrystallized from cyclohexane, to give 4-bromo-2-methoxyphenyl benzoate (22.7), m.p. 73°-75° C. [Elemental analysis: C,55.0; H,3.6; Br, 25.5%; calculated: C,54.6; H,3.9; Br, 25.9%]. The mixture is concentrated in vacuo the resulting residue is dissolved in methyl t-butyl ether (200 mL) washed with water (100 mL) and saturated aqueous sodium bicarbonate solution (3×100 mL) dried over magnesium sulphate evaporated The resulting residue is recrystallized from cyclohexane

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

実験手順: A stirred, ice-cold, aqueous solution of sodium hydroxide (250 mL; 15% w/v) is treated, dropwise, with guaiacol (22 mL), followed by benzoyl chloride (25.5 mL), and the mixture is stirred for a further period of 40 minutes. The resulting crystalline white solid is filtered off, washed with water, and dried, to give 2-methoxyphenyl benzoate (29.2 g), m.p. 59°-60° C. [Elemental analysis: C,73.3; H,5.2%; calculated: C,73.7; H,5.3%]. The resulting crystalline white solid is filtered off washed with water dried

反応条件: temp:2.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A stirred solution of 2-methoxyphenyl benzoate (10 g) in dichloromethane (100 mL) from 0-5° C. is treated dropwise with chlorosulfonic acid (2.9 mL) and the solution is then stirred for 3 hours from 0-5° C. The precipitate which forms is filtered off, washed with cold dichloromethane, and dried in vacuo, to give 3-benzoyloxy-4-methoxybenzenesulfonic acid (11.45 g), in the form of a white solid, m.p. 139-140° C. The precipitate which forms is filtered off washed with cold dichloromethane dried in vacuo

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

実験手順: A stirred solution of 2-methoxyphenyl benzoate (10 g) in dichloromethane (100 mL) from 0°-5° C. is treated dropwise with chlorosulfonic acid (2.9 mL) and the solution is then stirred for 3 hours from 0°-5° C. The precipitate which forms is filtered off, washed with cold dichloromethane, and dried in vacuo, to give 3-benzoyloxy-4-methoxybenzenesulfonic acid (11.45 g), in the form of a white solid, m.p. 139°-140° C. The precipitate which forms is filtered off washed with cold dichloromethane dried in vacuo

反応条件: temp:2.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A stirred solution of 2-methoxyphenyl benzoate (10 g) in dichloromethane (100 mL) from 0-5° C. is treated dropwise with chlorosulfonic acid (2.9 mL) and the solution is then stirred for 3 hours from 0-5° C. The precipitate which forms is filtered off, washed with cold dichloromethane, and dried in vacuo, to give 3-benzoyloxy-4-methoxybenzenesulfonic acid (11.45 g), in the form of a white solid, m.p. 139-140° C. The precipitate which forms is filtered off washed with cold dichloromethane dried in vacuo