Method for preparing 4-nitroso-substituted aromatic amine

[0048] Add 2.0 g (34 mmol) of acetamide, 4.1 g (68 mmol) of potassium hydroxide, 10 g of anhydrous potassium carbonate, 200 mg of pyrene and 15 ml of DMSO into a 100 ml reactor equipped with a condenser and a thermometer , and the mixture was heated with stirring in an oxygen atmosphere. When the reaction temperature reached 85° C., 1.4 g (11 mmol) of nitrobenzene was added dropwise through the dropping funnel for about 10 minutes. An extreme caution was employed in case the temperature inside the reactor might exceed 85±4°C. The time point at which nitrobenzene disappeared was determined as the end point of the reaction using HPLC. After reacting for 2 hours, DMSO was added to a predetermined amount of reactant, diluted with ethyl acetate, and then analyzed by HPLC.

[0049] The conversion of nitrobenzene was 100%. According to quantitative analysis, the product yield based on internal standard pyrene was 61 mole % for 4-nitrosoaniline and 8 mole % for 4-nitrosoaniline.

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[0056] This example illustrates the results using different amides. The same procedure was carried out as described in Example 1, except that various amides as listed in Table 2 were used instead of acetamide. The results are listed in Table 2.

[0057] Amide

[0059] Operate in the same manner as described in Example 1, except that the amount of nitrobenzene based on acetamide is variable as listed in Table 3. The results are listed in Table 3.

[0060] Nitrobenzene / B