methyl ester of 7-hydroxyheptanoic acid

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

実験手順: 1.6 g of methyl 7-hydroxyheptanoate and 1.08 g of o-phenylenediamine were refluxed for 7 hours in 15 ml of 2:1 hydrochloric acid aqueous solution. The reaction mixture was cooled to room temperature, then adjusted to pH 8 with addition of aqueous NaHCO3 and extracted with ethyl acetate. The extract was dried over sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate) to obtain 0.9 g of the title compound (yield: 41%). extracted with ethyl acetate The extract was dried over sodium sulfate the solvent was evaporated under reduced pressure The resulting residue was purified by silica gel column chromatography (ethyl acetate)

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

実験手順: 1.6 g of methyl 7-hydroxyheptanoate and 1.08 g of o-phenylenediamine were refluxed for 7 hours in 15 ml of 2:1 hydrochloric acid aqueous solution. The reaction mixture was cooled to room temperature, then adjusted to pH 8 with addition of aqueous NaHCO3 and extracted with ethyl acetate. The extract was dried over sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate) to obtain 0.9 g of the title compound (yield: 41%). extracted with ethyl acetate The extract was dried over sodium sulfate the solvent was evaporated under reduced pressure The resulting residue was purified by silica gel column chromatography (ethyl acetate)

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

実験手順: 3,3,3-Trifluoropropanol (10 ml, 110 mmol), methyl 7-hydroxyheptanoate (133 mmol, 1.2 eq), triphenylphosphine (35 g, 133 mmol, 1.2 eq) are initially introduced in 37 ml of THF in a round-bottomed flask and introduced into an ultrasound bath for a few minutes in order to mix the substances. During the exposure to ultrasound, DIAD (26.5 ml, 133 mmol, 1.2 eq) is very slowly added dropwise (temperature rises), and the reaction mixture is left under ultrasound for 15 min. A TLC sample is taken and subsequently left in the ultrasound bath for a further 2 hours. introduced into an ultrasound bath for a few minutes in order to mix the substances subsequently left in the ultrasound bath for a further 2 hours

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

実験手順: 3,3,3-Trifluoropropanol (10 ml, 110 mmol), methyl 7-hydroxyheptanoate (133 mmol, 1.2 eq), triphenylphosphine (35 g, 133 mmol, 1.2 eq) are initially introduced in 37 ml of THF in a round-bottomed flask and introduced into an ultrasound bath for a few minutes in order to mix the substances. During the exposure to ultrasound, DIAD (26.5 ml, 133 mmol, 1.2 eq) is very slowly added dropwise (temperature rises), and the reaction mixture is left under ultrasound for 15 min. A TLC sample is taken and subsequently left in the ultrasound bath for a further 2 hours. introduced into an ultrasound bath for a few minutes in order to mix the substances subsequently left in the ultrasound bath for a further 2 hours

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

実験手順: 1.6 g of methyl 7-hydroxyheptanoate and 1.08 g of o-phenylenediamine were refluxed for 7 hours in 15 ml of 2:1 hydrochloric acid aqueous solution. The reaction mixture was cooled to room temperature, then adjusted to pH 8 with addition of aqueous NaHCO3 and extracted with ethyl acetate. The extract was dried over sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate) to obtain 0.9 g of the title compound (yield: 41%). extracted with ethyl acetate The extract was dried over sodium sulfate the solvent was evaporated under reduced pressure The resulting residue was purified by silica gel column chromatography (ethyl acetate)

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

実験手順: 3,3,3-Trifluoropropanol (10 ml, 110 mmol), methyl 7-hydroxyheptanoate (133 mmol, 1.2 eq), triphenylphosphine (35 g, 133 mmol, 1.2 eq) are initially introduced in 37 ml of THF in a round-bottomed flask and introduced into an ultrasound bath for a few minutes in order to mix the substances. During the exposure to ultrasound, DIAD (26.5 ml, 133 mmol, 1.2 eq) is very slowly added dropwise (temperature rises), and the reaction mixture is left under ultrasound for 15 min. A TLC sample is taken and subsequently left in the ultrasound bath for a further 2 hours. introduced into an ultrasound bath for a few minutes in order to mix the substances subsequently left in the ultrasound bath for a further 2 hours