| 摘要 |
Preparation of sulfonamides of metallic phthalocyanines(1) comprise treatment with chlorosulfonic acid and an agent such as thionyl chloride, to ensure a complete conversion of all sulfonic acid groups, followed by amination in a single stage to obtain a maximum yield of the sulfonamide. Preparation of a metallic phthalocyanine sulfonamide catalyst of formula (1). MPc(SO2NHR)x (1) MPc = phthalocyanine of structure MPc; M = Co, Ni, Fe, Mn, Cr or V; x = 1, 2, 3 or 4; and R = H, alkyl or cycloalkyl. The process comprises the following stages: (1) Reaction of a metallic phthalocyanine with chlorosulfonic acid at 90 - 150 deg C for 1 - 5 hours; (2) Cooling of the mixture to 40 - 80 deg C; (3) Addition of 1 - 7 parts of a chloride reactant to the mixture; (4) Heating of the mixture obtained to 60 - 80 deg C for 0.5 - 3 hours to obtain the sulfonyl chloride; (5) Separation of the compound by adding the reaction mixture to ice/water; (6) Reaction of the sulfonyl chloride with an amine of formula (2). H2NHR (2) R = H, aryl, alkyl or cycloalkyl, in an aqueous or non-aqueous medium or mixture at -4 to 15 deg C and at a pH of 7 - 9, in the presence of an acid fixation agent, to give the required catalyst. |
