Method for preparing N,N-diethyl-3-pyridine carboxamide

[0019] Put 12.3g (about 0.1mol) of nicotinic acid and 128 ml of dichloromethane into the reaction bottle, stir, and put the reaction bottle into ice water to control the temperature at 0°C, and slowly add 12.8 ml of oxalyl chloride dropwise. , kept stirring at 0°C for 0.5~1h, then warmed up to room temperature, reacted for 4~6h, after the reaction was completed, 30% sodium hydroxide solution was added dropwise to adjust the pH of the reaction solution to 7, and then the temperature of the reaction mixture was controlled at -5~10°C to slowly Add 15.5ml of diethylamine dropwise. After the dropwise addition, react at room temperature for 6~8h. After the reaction is completed, add 17ml of 25% sodium carbonate solution. After stirring, let it stand for stratification, separate the lower water layer, and dry the organic layer. To obtain the crude product of N,N-diethyl-3-pyridinecarboxamide, add the crude product of N,N-diethyl-3-pyridinecarboxamide into dichloromethane, decolorize, oxi

[0021] Put 12.3g (about 0.1mol) of nicotinic acid and 160 ml of dichloromethane into the reaction bottle, stir, and put the reaction bottle into ice water to control the temperature at 0°C after stirring, and slowly add 15.4 ml of oxalyl chloride dropwise. , kept stirring at 0°C for 0.5~1h, then warmed up to room temperature, reacted for 4~6h, after the reaction was completed, 30% sodium hydroxide solution was added dropwise to adjust the pH of the reaction solution to 7, and then the temperature of the reaction mixture was controlled at -5~10°C to slowly Add 19.5ml of diethylamine dropwise. After the dropwise addition, react at room temperature for 6~8h. After the reaction is completed, add 20ml of 25% sodium carbonate solution. After stirring, let it stand for stratification. Separate the lower water layer and dry the organic layer. To obtain the crude product of N,N-diethyl-3-pyridinecarboxamide, add the crude product of N,N-diethyl-3-pyridinecarboxamide into dichloromethane, d

[0023] Put 12.3g (about 0.1mol) of nicotinic acid and 190 ml of dichloromethane into the reaction bottle, stir, and put the reaction bottle into ice water to control the temperature at 0°C after stirring, and slowly add 25 ml of oxalyl chloride dropwise. , kept stirring at 0°C for 0.5~1h, then warmed up to room temperature, reacted for 4~6h, after the reaction was completed, 30% sodium hydroxide solution was added dropwise to adjust the pH of the reaction solution to 7, and then the temperature of the reaction mixture was controlled at -5~10°C to slowly Add 30 ml of diethylamine dropwise. After the dropwise addition, react at room temperature for 6~8 hours. After the reaction is completed, add 33 ml of 25% sodium carbonate solution. After stirring, let stand to separate and separate the lower water layer, and dry the organic layer. To obtain the crude product of N,N-diethyl-3-pyridinecarboxamide, add the crude product of N,N-diethyl-3-pyridinecarboxamide into dichloromethane, deco