反应详情

温度

50 °C

A commercially available activated carbon-supported palladium catalyst “PDC-3000” available from Toyo C.C.I. Co., Ltd. (supported palladium: 3% by weight) was activated by reduction with hydrogen. A 100-ml autoclave was successively charged with 3.0 g of the activated catalyst, 12.8 g of isophthalonitrile containing as impurities 3.42% by weight of 3-cyanobenzamide and 0.24% by weight of 3-cyanobenzoic acid, 37 g of liquid ammonia, and 0.1 g of sodium hydroxide. Then, hydrogen was introduced into the autoclave to increase the inner pressure to 20 MPa (gauge). The concentration in the reaction solution was 0.877% by weight for the benzamide compound and 0.062% by weight for the benzoic acid compound. The autoclave was shaken at 50° C. for 30 min. The gas chromatographic analysis on the reaction product solution showed that the conversion of isophthalonitrile was 92.0 mol %, the yields of 3-cyanobenzylamine was 54.3 mol %, and the yield of m-xylylenediamine was 4.2 mol %. The by-products were substantially high-boiling substances.

1. temperatureto increase the inner pressure to 20 MPa (gauge)
2. concentrationThe concentration in the reaction solution