ethyl 4,4,4-trichloro-3-oxobutanoate

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: 3-Nitrobenzaldehyde (7.55 g, 50 mmoles), ethyl 4,4,4-trichloro-3-oxobutanoate (18.33 g, 59.5 mmoles), piperidine (0.66 ml) and hexanoic acid (0.33 ml) were heated at reflux in toluene (130 ml) for 48 hours using a Dean and Stark apparatus. The mixture was cooled, evaporated to dryness in vacuo and crystallised by trituration with ethyl acetate/petroleum ether (60°-80°). Recrystallisation from 2-propanol gave the sub-title compound (5.3 g) mp 105.5°-7°. The mixture was cooled evaporated to dryness in vacuo crystallised by trituration with ethyl acetate/petroleum ether (60°-80°) Recrystallisation from 2-propanol

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

実験手順: 4,4,4-Trichloro-3-oxo-butyric acid ethyl ester (Int 8, 1 eq) and H2NNH2.HCl (1.1 eq) are mixed in EtOH. The resulting mixture is refluxed overnight. The mixture is then evaporated and the obtained crude is purified by chromatography to give Int 9 and 5-ethoxy-2H-pyrazole-3-carboxylic acid ethyl ester (Int 10). The resulting mixture is refluxed overnight The mixture is then evaporated the obtained crude is purified by chromatography

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

実験手順: 3-Nitrobenzaldehyde (7.55 g, 50 mmoles), ethyl 4,4,4-trichloro-3-oxobutanoate (18.33 g, 59.5 mmoles), piperidine (0.66 ml) and hexanoic acid (0.33 ml) were heated at reflux in toluene (130 ml) for 48 hours using a Dean and Stark apparatus. The mixture was cooled, evaporated to dryness in vacuo and crystallised by trituration with ethyl acetate/petroleum ether (60°-80°). Recrystallisation from 2-propanol gave the sub-title compound (5.3 g) mp 105.5°-7°. The mixture was cooled evaporated to dryness in vacuo crystallised by trituration with ethyl acetate/petroleum ether (60°-80°) Recrystallisation from 2-propanol

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

実験手順: 3-Nitrobenzaldehyde (7.55 g, 50 mmoles), ethyl 4,4,4-trichloro-3-oxobutanoate (18.33 g, 59.5 mmoles), piperidine (0.66 ml) and hexanoic acid (0.33 ml) were heated at reflux in toluene (130 ml) for 48 hours using a Dean and Stark apparatus. The mixture was cooled, evaporated to dryness in vacuo and crystallised by trituration with ethyl acetate/petroleum ether (60°-80°). Recrystallisation from 2-propanol gave the sub-title compound (5.3 g) mp 105.5°-7°. The mixture was cooled evaporated to dryness in vacuo crystallised by trituration with ethyl acetate/petroleum ether (60°-80°) Recrystallisation from 2-propanol

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: 4,4,4-Trichloro-3-oxo-butyric acid ethyl ester (Int 8, 1 eq) and H2NNH2.HCl (1.1 eq) are mixed in EtOH. The resulting mixture is refluxed overnight. The mixture is then evaporated and the obtained crude is purified by chromatography to give Int 9 and 5-ethoxy-2H-pyrazole-3-carboxylic acid ethyl ester (Int 10). The resulting mixture is refluxed overnight The mixture is then evaporated the obtained crude is purified by chromatography

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

実験手順: 4,4,4-Trichloro-3-oxo-butyric acid ethyl ester (Int 8, 1 eq) and H2NNH2.HCl (1.1 eq) are mixed in EtOH. The resulting mixture is refluxed overnight. The mixture is then evaporated and the obtained crude is purified by chromatography to give Int 9 and 5-ethoxy-2H-pyrazole-3-carboxylic acid ethyl ester (Int 10). The resulting mixture is refluxed overnight The mixture is then evaporated the obtained crude is purified by chromatography

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

実験手順: 4,4,4-Trichloro-3-oxo-butyric acid ethyl ester (Int 8, 1 eq) and H2NNH2.HCl (1.1 eq) are mixed in EtOH. The resulting mixture is refluxed overnight. The mixture is then evaporated and the obtained crude is purified by chromatography to give Int 9 and 5-ethoxy-2H-pyrazole-3-carboxylic acid ethyl ester (Int 10). The resulting mixture is refluxed overnight The mixture is then evaporated the obtained crude is purified by chromatography

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

実験手順: 3-Nitrobenzaldehyde (7.55 g, 50 mmoles), ethyl 4,4,4-trichloro-3-oxobutanoate (18.33 g, 59.5 mmoles), piperidine (0.66 ml) and hexanoic acid (0.33 ml) were heated at reflux in toluene (130 ml) for 48 hours using a Dean and Stark apparatus. The mixture was cooled, evaporated to dryness in vacuo and crystallised by trituration with ethyl acetate/petroleum ether (60°-80°). Recrystallisation from 2-propanol gave the sub-title compound (5.3 g) mp 105.5°-7°. The mixture was cooled evaporated to dryness in vacuo crystallised by trituration with ethyl acetate/petroleum ether (60°-80°) Recrystallisation from 2-propanol