A kind of alkyl ketone amide and its oxime amide compound and its preparation and application
A technology for alkyl ketone amides and compounds, which is applied in the fields of alkyl ketone amides and oxime amide compounds and their preparation and application, can solve the problems such as the inability to smoothly introduce a single fluorine atom, and achieves improved application value and better reaction yield. rate effect
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Embodiment 1
[0055]
[0056] Synthesis of III1: Add 11.0g (125mmol) of pyruvic acid and 300mL of dichloromethane into a 1L round bottom flask, cool to 0°C, add dropwise 16.5g (130mmol) of oxalyl chloride, and 10 drops of N,N-dimethylformamide . The reaction was stirred at room temperature for 4 h, and then the solvent and excess oxalyl chloride were distilled off under reduced pressure. The residue was dissolved in 400 mL of toluene, and then 9.15 g (50 mmol) of pentafluoroaniline was added, and the resulting mixture was refluxed for 30 minutes, and the end point of the reaction was detected by TLC. The reaction was cooled to room temperature, and the toluene was distilled off under reduced pressure. The residue was dissolved in 100 mL of dichloromethane, washed three times with 100 mL of water, dried over sodium sulfate, filtered, and concentrated to obtain 11.0 g (87% yield) of yellow crude product III1. The crude product can be directly used in the next reaction.
[0057] Synthesis...
Embodiment 2
[0059]
[0060] Synthesis of III2: Add 5.3g (60mmol) of pyruvic acid and 300mL of dichloromethane into a 1L round bottom flask, cool to 0°C, add dropwise 9.1g (72mmol) of oxalyl chloride, 10 drops of N,N-dimethylformamide . The reaction was stirred at room temperature for 4 h, and then the solvent and excess oxalyl chloride were distilled off under reduced pressure. The residue was dissolved in 400 mL of toluene, and then 5.0 g (50 mmol) of cyclohexylamine was added, and the resulting mixture was refluxed for 30 minutes, and the end point of the reaction was detected by TLC. The reaction was cooled to room temperature, and the toluene was distilled off under reduced pressure. The residue was dissolved in 100 mL of dichloromethane, washed three times with 100 mL of water, dried over sodium sulfate, filtered, and concentrated to obtain 27.4 g (87% yield) of yellow crude product III. The crude product can be directly used in the next reaction.
[0061] Synthesis of IV2: 26.8...
Embodiment 3
[0063]
[0064] Synthesis of III3: Add 5.3g (60mmol) of pyruvic acid and 300mL of dichloromethane into a 1L round bottom flask, cool to 0°C, add dropwise 10.7g (90mmol) of thionyl chloride, N,N-dimethylformamide 10 drops. The reaction was stirred at room temperature for 4 h, and then the solvent and excess thionyl chloride were distilled off under reduced pressure. The residue was dissolved in 400 mL of toluene, and then 4.7 g (50 mmol) of aniline was added, and the resulting mixture was refluxed for 30 minutes, and the end point of the reaction was detected by TLC. The reaction was cooled to room temperature, and the toluene was distilled off under reduced pressure. The residue was dissolved in 100 mL of dichloromethane, washed three times with 100 mL of water, dried over sodium sulfate, filtered, and concentrated to give 37.3 g (90% yield) of yellow crude product III. The crude product can be directly used in the next reaction.
[0065] Synthesis of IV3: 36.5g (40mmol) ...
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