反应详情

温度

70 °C

85 Parts of an aqueous solution of technical sodium hydrosulfide containing 35 percent NaHS and 9 percent Na2S 2 O3 were added to a mixture comprising 65.4 parts of 2,2'-dichlor-5,5'-dichloroazoxybenzene in 196 parts of methanol at room temperature within 90 minutes. The reaction mixture was then refluxed at 70° C to75° C for a period of 5 hours. The pH had been kept between 9 and 9.4. After this period the starting azoxybenzene was shown to be all consumed and the reaction mixture was cooled down to 0° C to 5° C, and the resulting precipitate filtered off and washed with water until alkali-free. After drying below 70° C 48 parts of 2,2'-dichloro,-5,5'-dichlorohydrazobenzene of a melting point of 116° C were obtained, this representing yield of 76 percent of the theory.

1. customat room temperature
2. customwithin 90 minutes
3. customall consumed
4. temperaturethe reaction mixture was cooled down to 0° C to 5° C
5. filtrationthe resulting precipitate filtered off
6. washwashed with water until alkali-free
7. customAfter drying below 70° C 48 parts of 2,2'-dichloro