Dimethyl 5-aminoisophthalate

13290-96-5

99-27-4

The general procedure for the synthesis of dimethyl 5-aminoisophthalate from dimethyl 5-nitroisophthalate was as follows: the hydrogenation of nitroaromatics was carried out in a PTFE-lined stainless steel autoclave equipped with a manometer and a magnetic stirrer. The procedure was as follows: 0.5 mmol of dimethyl 5-nitroisophthalate, 15 mol% of Co/C-N-X catalyst, 100 μL of n-hexadecane, and 2 mL of solvent were mixed and added to the reactor at room temperature. The autoclave was purged several times using hydrogen to remove air. After the preset reaction temperature was reached, the hydrogen pressure was adjusted to 1 MPa and a magnetic stirrer (600 r/min) was activated to start the reaction. Upon completion of the reaction, the solid catalyst in the reaction solution was separated by centrifugation. The products in the reaction solution were quantitatively analyzed and structurally identified by gas chromatography-mass spectrometry (Shimadzu GCMS-QP5050A, equipped with a 0.25 mm × 30 m DB-WAX capillary column). Nuclear magnetic resonance hydrogen (1H NMR) and carbon (13C NMR) spectral data were acquired on a Bruker Avance III 400 spectrometer using CDCl3 or DMSO-d6 as solvents and tetramethylsilane (TMS) as an internal standard. Pure products from amplification experiments were obtained by fast column chromatography (eluent was a solvent mixture of petroleum ether and ethyl acetate) purification.