1. Preparation of raw materials: weigh 20 g of isobutyl 3,5-dinitro-4-chlorobenzoate, 100 ml of ethanol, 4 g of nickel ruanne and 1 g of morpholine.
2. Procedure:
1) Add the weighed isobutyl 3,5-dinitro-4-chlorobenzoate, nickel ruanne, ethanol and morpholine into the autoclave, seal it, and then replace the gas in the autoclave with nitrogen and hydrogen at 0.2-0.3 MPa, respectively, and repeat the process 3 times each;
2) pass hydrogen into the autoclave until the pressure reaches 3.0 MPa, heat to 90-100°C and maintain this temperature until the pressure in the kettle drops to 2.0 MPa, and then replenish hydrogen to 3.0 MPa;
3) Maintaining the pressure in the reactor between 2.0-3.0 MPa and continuing the reaction for 1.5 hours until the system no longer absorbs hydrogen and the reaction is complete, stopping heating and cooling;
4) After the completion of the reaction, carry out filtration to recover the solid Nguyenne nickel;
5) Concentrate the filtrate under reduced pressure to a viscous state, and then place it in a refrigerator for freeze crystallization.
3. Experimental results: The reaction was successfully completed with 92% yield of isobutyl 4-chloro-3,5-diaminobenzoate.
