反应详情

温度

75 °C

84 Parts of an aqueous solution of technical sodium hydrosulfide, free from sodium thiosulphate, were added to a mixture comprising 53.4 parts of 2,2'-dichloroazoxybenzene in 140 parts of morpholine at 60° C - 65° C within 90 minutes. Subsequently, the reaction temperature was raised to 75° C and maintained at that temperature for 2 1/2 hours. Next the temperature was further raised to 90° C and maintained at that temperature for 1 hour. The pH of the reaction mixture varied between 9.5 to 10. After this period the absence of the starting material was confirmed. Then the reaction mixture was cooled to 20° C and neutralized cautiously with 400 parts of hydrochloric acid of 15 percent strength at a temperature below 20° C. Then the reaction mixture was cooled to 0° C to 5° C, and the resulting precipiatate filtered off and washed with water until free of chloride. After drying below 70° C, 40.1 parts of 2,2'-dichlorohydrazobenzene of a melting point of 85° C to 87° C were obtained, this representing a yield of 79 percent of the theory.

1. customat 60° C - 65° C
2. customwithin 90 minutes
3. temperaturemaintained at that temperature for 2 1/2 hours
4. temperatureNext the temperature was further raised to 90° C
5. temperaturemaintained at that temperature for 1 hour
6. waitAfter this period the absence of the starting material was confirmed
7. temperatureThen the reaction mixture was cooled to 0° C to 5° C
8. filtrationthe resulting precipiatate filtered off
9. washwashed with water until free of chloride
10. customAfter drying below 70° C