preparation | add 28.129(0.2mol)3-bromobenzaldehyde, 29.129(0.28mol) malonic acid, 3.3mL piperidine and 120mL ethanol into an autoclave with a volume of 500mL, tighten the autoclave, check the air tightness, and replace the air in the autoclave with nitrogen. When the pressure rises to 0.6~0.8 MPa, start heating and stirring. The reaction temperature was controlled at 95 ℃ for 10h. The pressure will gradually increase at the beginning of the reaction, and the pressure will decrease at the end of the reaction. When the pressure of the autoclave is unchanged, the reaction is stopped, the reaction mixture is cooled to room temperature, and the filtration is carried out. Wash the solid with 50mL distilled water and dry it to obtain 31.69 white powder product. |