ethyl 2,3-dihydroxybenzoate

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

実験手順: To a solution of 2,3-dihydroxybenzoic acid (25 g) in ethanol (320 ml) was added concentrated sulfuric acid (1.8 ml), and the mixture was heated under reflux for one day. The reaction mixture was concentrated, poured into water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to normal phase chromatography (elution solvent ethyl acetate) to give the title compound (30 g, 100%). the mixture was heated under reflux for one day The reaction mixture was concentrated poured into water the mixture was extracted with ethyl acetate The organic layer was washed with saturated brine dried over sodium sulfate The solvent was evaporated under reduced pressure The residue was subjected to normal phase chromatography (elution solvent ethyl acetate)

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

実験手順: A mixture of 2,3-dihydroxybenzoic acid(994 g), ethanol (3.8 L) and sulfuric acid (320 g) was refluxed for 44 hours. A portion of the solvent distilled out of the solution, and the solution was cooled and stirred overnight, and then further cooled in an ice/water bath. To the solution was added water (5.6 L). The solution was aged, and the crystals were filtered, washed with water, and dried to give ethyl 2,3-dihydroxybenzoate (1002 g, 85%); m.p. 66.0-67.2° C. was refluxed for 44 hours A portion of the solvent distilled out of the solution the solution was cooled further cooled in an ice/water bath To the solution was added water (5.6 L) the crystals were filtered washed with water dried

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

実験手順: A mixture of 2,3-dihydroxybenzoic acid(994 g), ethanol (3.8 L) and sulfuric acid (320 g) was refluxed for 44 hours. A portion of the solvent distilled out of the solution, and the solution was cooled and stirred overnight, and then further cooled in an ice/water bath. To the solution was added water (5.6 L). The solution was aged, and the crystals were filtered, washed with water, and dried to give ethyl 2,3-dihydroxybenzoate (1002 g, 85%); m.p. 66.0-67.2° C. was refluxed for 44 hours A portion of the solvent distilled out of the solution the solution was cooled further cooled in an ice/water bath To the solution was added water (5.6 L) the crystals were filtered washed with 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 2,3-dihydroxybenzoic acid (25 g) in ethanol (320 ml) was added concentrated sulfuric acid (1.8 ml), and the mixture was heated under reflux for one day. The reaction mixture was concentrated, poured into water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to normal phase chromatography (elution solvent ethyl acetate) to give the title compound (30 g, 100%). the mixture was heated under reflux for one day The reaction mixture was concentrated poured into water the mixture was extracted with ethyl acetate The organic layer was washed with saturated brine dried over sodium sulfate The solvent was evaporated under reduced pressure The residue was subjected to normal phase chromatography (elution solvent ethyl acetate)

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

実験手順: A mixture of 2,3-dihydroxybenzoic acid(994 g), ethanol (3.8 L) and sulfuric acid (320 g) was refluxed for 44 hours. A portion of the solvent distilled out of the solution, and the solution was cooled and stirred overnight, and then further cooled in an ice/water bath. To the solution was added water (5.6 L). The solution was aged, and the crystals were filtered, washed with water, and dried to give ethyl 2,3-dihydroxybenzoate (1002 g, 85%); m.p. 66.0-67.2° C. was refluxed for 44 hours A portion of the solvent distilled out of the solution the solution was cooled further cooled in an ice/water bath To the solution was added water (5.6 L) the crystals were filtered washed with 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 2,3-dihydroxybenzoic acid (25 g) in ethanol (320 ml) was added concentrated sulfuric acid (1.8 ml), and the mixture was heated under reflux for one day. The reaction mixture was concentrated, poured into water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to normal phase chromatography (elution solvent ethyl acetate) to give the title compound (30 g, 100%). the mixture was heated under reflux for one day The reaction mixture was concentrated poured into water the mixture was extracted with ethyl acetate The organic layer was washed with saturated brine dried over sodium sulfate The solvent was evaporated under reduced pressure The residue was subjected to normal phase chromatography (elution solvent ethyl acetate)